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Evaluation of the X-ray/EUV Nanolithography Facility at AS through wavefront propagation simulations

Synchrotron light sources can provide the required spatial coherence, stability and control to support the development of advanced lithography at the extreme ultraviolet and soft X-ray wavelengths that are relevant to current and future fabricating technologies. Here an evaluation of the optical performance of the soft X-ray (SXR) beamline of the Australian Synchrotron (AS) and its suitability for developing interference lithography using radiation in the 91.8 eV (13.5 nm) to 300 eV (4.13 nm) range are presented. A comprehensive physical optics model of the APPLE-II undulator source and SXR beamline was constructed to simulate the properties of the illumination at the proposed location of a photomask, as a function of photon energy, collimation and monochromator parameters. The model is validated using a combination of experimental measurements of the photon intensity distribution of the undulator harmonics. It is shown that the undulator harmonics intensity ratio can be accurately measured using an imaging detector and controlled using beamline optics. Finally, the photomask geometric constraints and achievable performance for the limiting case of fully spatially coherent illumination are evaluated.




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Operando double-edge high-resolution X-ray absorption spectroscopy study of BiVO4 photoanodes

High energy resolution fluorescence detected X-ray absorption spectroscopy is a powerful method for probing the electronic structure of functional materials. The X-ray penetration depth and photon-in/photon-out nature of the method allow operando experiments to be performed, in particular in electrochemical cells. Here, operando high-resolution X-ray absorption measurements of a BiVO4 photoanode are reported, simultaneously probing the local electronic states of both cations. Small but significant variations of the spectral lineshapes induced by the applied potential were observed and an explanation in terms of the occupation of electronic states at or near the band edges is proposed.




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Laminography as a tool for imaging large-size samples with high resolution

Despite the increased brilliance of the new generation synchrotron sources, there is still a challenge with high-resolution scanning of very thick and absorbing samples, such as a whole mouse brain stained with heavy elements, and, extending further, brains of primates. Samples are typically cut into smaller parts, to ensure a sufficient X-ray transmission, and scanned separately. Compared with the standard tomography setup where the sample would be cut into many pillars, the laminographic geometry operates with slab-shaped sections significantly reducing the number of sample parts to be prepared, the cutting damage and data stitching problems. In this work, a laminography pipeline for imaging large samples (>1 cm) at micrometre resolution is presented. The implementation includes a low-cost instrument setup installed at the 2-BM micro-CT beamline of the Advanced Photon Source. Additionally, sample mounting, scanning techniques, data stitching procedures, a fast reconstruction algorithm with low computational complexity, and accelerated reconstruction on multi-GPU systems for processing large-scale datasets are presented. The applicability of the whole laminography pipeline was demonstrated by imaging four sequential slabs throughout an entire mouse brain sample stained with osmium, in total generating approximately 12 TB of raw data for reconstruction.




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3D imaging of magnetic domains in Nd2Fe14B using scanning hard X-ray nanotomography

Nanoscale structural and electronic heterogeneities are prevalent in condensed matter physics. Investigating these heterogeneities in 3D has become an important task for understanding material properties. To provide a tool to unravel the connection between nanoscale heterogeneity and macroscopic emergent properties in magnetic materials, scanning transmission X-ray microscopy (STXM) is combined with X-ray magnetic circular dichroism. A vector tomography algorithm has been developed to reconstruct the full 3D magnetic vector field without any prior noise assumptions or knowledge about the sample. Two tomographic scans around the vertical axis are acquired on single-crystalline Nd2Fe14B pillars tilted at two different angles, with 2D STXM projections recorded using a focused 120 nm X-ray beam with left and right circular polarization. Image alignment and iterative registration have been implemented based on the 2D STXM projections for the two tilts. Dichroic projections obtained from difference images are used for the tomographic reconstruction to obtain the 3D magnetization distribution at the nanoscale.




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High-throughput and high-resolution powder X-ray diffractometer consisting of six sets of 2D CdTe detectors with variable sample-to-detector distance and innovative automation system

The demand for powder X-ray diffraction analysis continues to increase in a variety of scientific fields, as the excellent beam quality of high-brightness synchrotron light sources enables the acquisition of high-quality measurement data with high intensity and angular resolution. Synchrotron powder diffraction has enabled the rapid measurement of many samples and various in situ/operando experiments in nonambient sample environments. To meet the demands for even higher throughput measurements using high-energy X-rays at SPring-8, a high-throughput and high-resolution powder diffraction system has been developed. This system is combined with six sets of two-dimensional (2D) CdTe detectors for high-energy X-rays, and various automation systems, including a system for automatic switching among large sample environmental equipment, have been developed in the third experimental hutch of the insertion device beamline BL13XU at SPring-8. In this diffractometer system, high-brilliance and high-energy X-rays ranging from 16 to 72 keV are available. The powder diffraction data measured under ambient and various nonambient conditions can be analysed using Rietveld refinement and the pair distribution function. Using the 2D CdTe detectors with variable sample-to-detector distance, three types of scan modes have been established: standard, single-step and high-resolution. A major feature is the ability to measure a whole powder pattern with millisecond resolution. Equally important, this system can measure powder diffraction data with high Q exceeding 30 Å−1 within several tens of seconds. This capability is expected to contribute significantly to new research avenues using machine learning and artificial intelligence by utilizing the large amount of data obtained from high-throughput measurements.




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Dual-beam X-ray nano-holotomography

Nanotomography with hard X-rays is a widely used technique for high-resolution imaging, providing insights into the structure and composition of various materials. In recent years, tomographic approaches based on simultaneous illuminations of the same sample region from different angles by multiple beams have been developed at micrometre image resolution. Transferring these techniques to the nanoscale is challenging due to the loss in photon flux by focusing the X-ray beam. We present an approach for multi-beam nanotomography using a dual-beam Fresnel zone plate (dFZP) in a near-field holography setup. The dFZP generates two nano-focused beams that overlap in the sample plane, enabling the simultaneous acquisition of two projections from slightly different angles. This first proof-of-principle implementation of the dual-beam setup allows for the efficient removal of ring artifacts and noise using machine-learning approaches. The results open new possibilities for full-field multi-beam nanotomography and pave the way for future advancements in fast holotomography and artifact-reduction techniques.




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Roentgenoscopy of laser-induced projectile impact testing

Laser-induced projectile impact testing (LIPIT) based on synchrotron imaging is proposed and validated. This emerging high-velocity, high-strain microscale dynamic loading technique offers a unique perspective on the strain and energy dissipation behavior of materials subjected to high-speed microscale single-particle impacts. When combined with synchrotron radiation imaging techniques, LIPIT allows for in situ observation of particle infiltration. Two validation experiments were carried out, demonstrating the potential of LIPIT in the roentgenoscopy of the dynamic properties of various materials. With a spatial resolution of 10 µm and a temporal resolution of 33.4 µs, the system was successfully realized at the Beijing Synchrotron Radiation Facility 3W1 beamline. This innovative approach opens up new avenues for studying the dynamic properties of materials in situ.




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Signal-to-noise and spatial resolution in in-line imaging. 1. Basic theory, numerical simulations and planar experimental images

Signal-to-noise ratio and spatial resolution are quantitatively analysed in the context of in-line (propagation based) X-ray phase-contrast imaging. It is known that free-space propagation of a coherent X-ray beam from the imaged object to the detector plane, followed by phase retrieval in accordance with Paganin's method, can increase the signal-to-noise in the resultant images without deteriorating the spatial resolution. This results in violation of the noise-resolution uncertainty principle and demonstrates `unreasonable' effectiveness of the method. On the other hand, when the process of free-space propagation is performed in software, using the detected intensity distribution in the object plane, it cannot reproduce the same effectiveness, due to the amplification of photon shot noise. Here, it is shown that the performance of Paganin's method is determined by just two dimensionless parameters: the Fresnel number and the ratio of the real decrement to the imaginary part of the refractive index of the imaged object. The relevant theoretical analysis is performed first, followed by computer simulations and then by a brief test using experimental images collected at a synchrotron beamline. More extensive experimental tests will be presented in the second part of this paper.




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Mango wiggler as a novel insertion device providing a large and symmetrical imaging field of view

A novel insertion device is introduced, designated as the Mango wiggler, designed for synchrotron radiation (SR) imaging that provides a large field of view. This innovative device is constructed from two orthogonal planar wigglers with a small difference in their period lengths, eliciting the phase difference of the magnetic fields to incrementally transitions from 0 to π/2. Such a configuration enlarges the vertical divergence of the light source, as with the horizontal divergence. The appellation `Mango wiggler' derives from the distinctive mango-shaped contour of its radiation field. A comprehensive suite of theoretical analyses and simulations has been executed to elucidate the radiation properties of the Mango wiggler, employing SPECTRA and Mathematica as calculation tools. In conjunction with the ongoing construction of the High Energy Photon Source in Beijing a practical Mango wiggler device has been fabricated for utilization in SR imaging applications. Theoretical analyses were applied to this particular Mango wiggler to yield several theoretical conclusions, and several simulations were performed according to the measured magnetic field results.




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Sub-nanometre quality X-ray mirrors created using ion beam figuring

Ion beam figuring (IBF) is a powerful technique for figure correction of X-ray mirrors to a high accuracy. Here, recent technical advancements in the IBF instrument developed at Diamond Light Source are presented and experimental results for figuring of X-ray mirrors are given. The IBF system is equipped with a stable DC gridded ion source (120 mm diameter), a four-axis motion stage to manipulate the optic, a Faraday cup to monitor the ion-beam current, and a camera for alignment. A novel laser speckle angular measurement instrument also provides on-board metrology. To demonstrate the IBF system's capabilities, two silicon X-ray mirrors were processed. For 1D correction, a height error of 0.08 nm r.m.s. and a slope error of 44 nrad r.m.s. were achieved. For 2D correction over a 67 mm × 17 mm clear aperture, a height error of 0.8 nm r.m.s. and a slope error of 230 nrad r.m.s. were obtained. For the 1D case, this optical quality is comparable with the highest-grade, commercially available, X-ray optics.




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Nonlinear optimization for a low-emittance storage ring

A multi-objective genetic algorithm (MOGA) is a powerful global optimization tool, but its results are considerably affected by the crossover parameter ηc. Finding an appropriate ηc demands too much computing time because MOGA needs be run several times in order to find a good ηc. In this paper, a self-adaptive crossover parameter is introduced in a strategy to adopt a new ηc for every generation while running MOGA. This new scheme has also been adopted for a multi-generation Gaussian process optimization (MGGPO) when producing trial solutions. Compared with the existing MGGPO and MOGA, the MGGPO and MOGA with the new strategy show better performance in nonlinear optimization for the design of low-emittance storage rings.




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Area normalization of HERFD-XANES spectra

The normalization of X-ray absorption near-edge structure (XANES) spectra is required for comparing spectral features and extracting quantitative information in analytical techniques such as linear combination analysis, principal component analysis and multivariate curve resolution. Most published data are normalized to the edge-jump, but normalization to the spectral area has also been applied. The latter is particularly attractive if only a small energy range around the absorption can be recorded reliably. Here, the two normalization methods are compared at the L3-edge of Pt, Pd and Rh, and at the Ni K-edge using experimental and calculated spectra. Normalization to the spectral area is found to be a viable approach if the range for the area normalization is sufficiently large.




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A versatile sample-delivery system for X-ray photoelectron spectroscopy of in-flight aerosols and free nanoparticles at MAX IV Laboratory

Aerosol science is of utmost importance for both climate and public health research, and in recent years X-ray techniques have proven effective tools for aerosol-particle characterization. To date, such methods have often involved the study of particles collected onto a substrate, but a high photon flux may cause radiation damage to such deposited particles and volatile components can potentially react with the surrounding environment after sampling. These and many other factors make studies on collected aerosol particles challenging. Therefore, a new aerosol sample-delivery system dedicated to X-ray photoelectron spectroscopy studies of aerosol particles and gas molecules in-flight has been developed at the MAX IV Laboratory. The aerosol particles are brought from atmospheric pressure to vacuum in a continuous flow, ensuring that the sample is constantly renewed, thus avoiding radiation damage, and allowing measurements on the true unsupported aerosol. At the same time, available gas molecules can be used for energy calibration and to study gas-particle partitioning. The design features of the aerosol sample-delivery system and important information on the operation procedures are described in detail here. Furthermore, to demonstrate the experimental range of the aerosol sample-delivery system, results from aerosol particles of different shape, size and composition are presented, including inorganic atmospheric aerosols, secondary organic aerosols and engineered nanoparticles.




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In situ characterization of stresses, deformation and fracture of thin films using transmission X-ray nanodiffraction microscopy. Corrigendum

Errors in variable subscripts, equations and Fig. 8 in Section 3.2 of the article by Lotze et al. [(2024). J. Synchrotron Rad. 31, 42–52] are corrected.




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Using convolutional neural network denoising to reduce ambiguity in X-ray coherent diffraction imaging

The inherent ambiguity in reconstructed images from coherent diffraction imaging (CDI) poses an intrinsic challenge, as images derived from the same dataset under varying initial conditions often display inconsistencies. This study introduces a method that employs the Noise2Noise approach combined with neural networks to effectively mitigate these ambiguities. We applied this methodology to hundreds of ambiguous reconstructed images retrieved from a single diffraction pattern using a conventional retrieval algorithm. Our results demonstrate that ambiguous features in these reconstructions are effectively treated as inter-reconstruction noise and are significantly reduced. The post-Noise2Noise treated images closely approximate the average and singular value decomposition analysis of various reconstructions, providing consistent and reliable reconstructions.




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A distributed software system for integrating data-intensive imaging methods in a hard X-ray nanoprobe beamline at the SSRF

The development of hard X-ray nanoprobe techniques has given rise to a number of experimental methods, like nano-XAS, nano-XRD, nano-XRF, ptychography and tomography. Each method has its own unique data processing algorithms. With the increase in data acquisition rate, the large amount of generated data is now a big challenge to these algorithms. In this work, an intuitive, user-friendly software system is introduced to integrate and manage these algorithms; by taking advantage of the loosely coupled, component-based design approach of the system, the data processing speed of the imaging algorithm is enhanced through optimization of the parallelism efficiency. This study provides meaningful solutions to tackle complexity challenges faced in synchrotron data processing.




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meso-α,α-5,15-Bis(o-nicotinamido­phen­yl)-10,20-diphen­ylporphyrin n-hexane monosolvate

The structure of the title solvated porphyrin, C56H38N8O2·C6H14, is reported. Two porphyrin mol­ecules, one ordered and one disordered n-hexane solvate mol­ecules are present in its asymmetric unit. The porphyrin macrocycle shows a characteristic saddle-shaped distortion, and the maximum deviation from the mean plane for non-hydrogen atoms is 0.48 Å. N—H⋯N, N—H⋯O, and C—H⋯O hydrogen bonds, as well as π–π inter­actions, are observed in the crystal structure.




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2-Amino­benzoxazole–oxalic acid (2/1)

In the title compound, 2C7H7N2O+·C2O42−, proton transfer from oxalic acid to the N atom of the heterocycle has occurred to form a 2:1 molecular salt. In the extended structure, N—H⋯O hydrogen bonds link the components into [100] chains, which feature R22(8) and R44(14) loops.




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Synthesis and structure of trans-bis­(4-amino-3-nitro­benzoato-κO)bis­(4-amino-3-nitro­benzoic acid-κO)di­aqua­manganese(II) dihydrate

The manganese title complex, [Mn(C7H5N2O4)2(C7H6N2O4)2(H2O)2]·2H2O, is one of the first 4-amino 3-nitro­benzoic acid (4 A3NBA) monoligand metal complexes to be synthesized. It crystallizes in the centrosymmetric monoclinic space group P21/n with the complex mol­ecules located on inversion centers. Four 4 A3NBA ligand mol­ecules are monodentately coordinated by the Mn2+ ion through the carb­oxy­lic oxygen atoms while the other two positions of the inner coordination sphere are occupied by water mol­ecules, giving rise to a distorted octa­hedron, and two water mol­ecules are in the outer coordination sphere. There are two intra­molecular hydrogen bonds in the complex mol­ecule. The first is of the common N—H⋯O=N type, while the second is a rarely occurring very strong hydrogen bond in which a common proton is shared by two uncoordinated oxygen atoms of neighboring carboxyl­ate groups. In the crystal, an intricate system of inter­molecular hydrogen bonds links the complex mol­ecules into a three-dimensional-network.




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Bis[2,6-bis­(benzimidazol-2-yl)pyridine-κ3N,N',N'']nickel(II) bis­(tri­fluoro­methane­sulfonate) diethyl ether monosolvate

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).




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Bis[μ-bis­(pyridin-2-yl)methanone oxime-κ3N:,N',N'']bis­[di­acetato-κ2O,O';κO-zinc(II)]

The structure of the title complex, [Zn2(C2H3O2)4(C11H9N3O)2], is triclinic containing half of the mol­ecule in the asymmetric unit. Each zinc atom is coordinated to a pyridyl and oxime nitro­gen from one di-2-pyridyl ketone oxime (dpko) ligand and a third nitro­gen from the other dpko pyridyl ring. Additionally, each zinc is coordinated to two acetato anions, one of which is bidentate and the other monodentate. The uncoordinated oxygen of the monodentate acetato group is involved in a hydrogen bond with the oxime hydrogen. The packing in the crystal is assisted by weak C—H⋯O inter­actions between acetato groups and neighboring pyridyl rings.




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1-Ethyl-3,3-di­methyl­spiro­[indoline-2,8'-phenaleno[1,9-fg]chromene]

The title pyrene-fused spiro­pyran derivative, C30H25NO, crystallizes with two mol­ecules in the asymmetric unit with dihedral angles between their fused-ring sub units of 76.20 (8) and 89.38 (9)°. In the crystal, weak C—H⋯π inter­actions link the mol­ecules into a three-dimensional network.




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4-Fluoro-2-(phenyl­amino)­benzoic acid

The title compound, C13H10FNO2, was obtained by the reaction of 2-bromo-4-fluoro­benzoic acid with aniline. There are two independent mol­ecules, A and B, in the asymmetric unit, with slight conformational differences: the dihedral angles between the aromatic rings are 55.63 (5) and 52.65 (5)°. Both mol­ecules feature an intra­molecular N—H⋯O hydrogen bond. In the crystal, the mol­ecules are linked by pairwise O—H⋯O hydrogen bonds to form A–B acid–acid dimers and weak C—H⋯F inter­actions further connect the dimers.




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5-Bromo-2-(phenyl­amino)­benzoic acid

The title compound, C13H10BrNO2, was obtained by the reaction of 2,5-di­bromo­benzoic acid and aniline. The mol­ecule is twisted with a dihedral angle between the aromatic rings of 45.74 (11)° and an intr­amolecular N—H⋯O hydrogen bond is seen. In the crystal, pairwise O—H⋯O hydrogen bonds generate carb­oxy­lic acid inversion dimers.




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Poly[(μ-2,3-diethyl-7,8-di­methyl­quinoxaline-κ2N:N)(2,3-diethyl-7,8-di­methyl­quinoxaline-κN)-μ-nitrato-κ2O:O'-nitrato-κ2O,O'-disilver(I)]

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.




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13-Nitro­benzo[a][1,4]benzo­thia­zino[3,2-c]phenoxazine

In the title compound, C22H11N3O3S, dihedral angle between the phenyl rings on the periphery of the molecule is 8.05 (18)°. In the crystal, aromatic π–π stacking distance and short C—H⋯O contacts are observed. The maximum absorption occurs at 688 nm.




no

Ethidium benzoate methanol monosolvate

In the title salt solvate (systematic name: 8-amino-5-ethyl-6-phenyl­phenanthridin-5-ium benzoate methanol monosolvate), C21H20N3+·C6H5CO2−·CH3OH, two ethidium cations, C21H20N3+, dimerize about a twofold axis through π–π inter­actions [inter-centroid separation = 3.6137 (4) Å]. The benzoate anions are connected through hydrogen bonding with the –NH2 groups of the ethidium cations and the –OH group of the MeOH mol­ecule. The MeOH mol­ecule also accepts a hydrogen bond from the –NH2 group of the ethidium cation. The result is a one-dimensional hydrogen-bonded chain along the b-axis direction.




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Bis[2,3-bis­(thio­phen-2-yl)pyrido[3,4-b]pyrazine]­silver(I) perchlorate methanol disolvate

The title compound, [Ag(C15H9N3S2)2]ClO4·2CH3OH, is monoclinic. The AgI atom is coordinated by pyrido N atoms and is two-coordinate; however, the AgI atom has nearby O atoms that can be assumed to be weakly bonded – one from the perchlorate anion and one from the methanol solvate molecule. One of the thienyl groups on a 2,3-bis­(thio­phen-2-yl)pyrido[3,4-b]pyrazine is flipped disordered and was refined to occupancies of 68.4 (6) and 31.6 (6)%.




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mer-Bis(quinoline-2-carboxaldehyde 4-ethyl­thio­semicarbazonato)nickel(II) methanol 0.33-solvate 0.67-hydrate

In the title compound, [Ni(C13H13N4S)2]·0.33CH3OH·0.67H2O, the NiII atom is coordinated by two tridentate quinoline-2-carboxaldehyde 4-ethyl­thio­semi­car­ba­zonate ligands in a distorted octa­hedral shape. At 100 K, the crystal symmetry is monoclinic (space group P21/n). A mixture of water and methanol crystallizes with the title complex, and one of the ethyl groups in the coordinating ligands is disordered over two positions, with an occupancy ratio of 58:42. There is inter­molecular hydrogen bonding between the solvent mol­ecules and the amine and thiol­ate groups in the ligands. No other significant inter­actions are present in the crystal packing.




no

Benzo[a][1,4]benzothia­zino[3,2-c]phenothia­zine

The title compound, C22H12N2S2, crystallizes in space group P21/c with four mol­ecules in the asymmetric unit. The heterocyclic mol­ecule is quasi-planar with a dihedral angle between the phenyl rings on the periphery of the mol­ecule of 1.73 (19)°. Short H⋯S (2.92 Å) and C—H⋯π [2.836 (3) Å] contacts are observed in the crystal with shorted π–π stacking distances of 3.438 (3) Å along the b axis. Surprisingly, and unlike a closely related material, this mol­ecule readily forms large crystals by sublimation and by slow evaporation from di­chloro­methane. The maximum absorbance in the UV-Vis spectrum is at 533 nm. Emission was measured upon excitation at 533 nm with a fluorescence λmax of 658 nm and cutoff of 900 nm.




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(2E,2'E)-1,1'-([1,1'-Biphen­yl]-4,4'-di­yl)bis­[3-(di­meth­yl­amino)­prop-2-en-1-one]

The title compound, C22H24N2O2, crystallizes in space group P21/n. The mol­ecular structure is almost planar except for a tilt of the phenyl rings. The allyl groups on both ends exhibit the trans-form and the connected N atoms show sp2 character. The mol­ecules are stacked and assembled along the c-axis direction by C—H⋯π inter­actions.




no

4-(1H-2,3-Dihydronaphtho­[1,8-de][1,3,2]di­aza­borinin-2-yl)-1-ethylpyridin-1-ium iodide monohydrate

The cation of the title hydrated salt, C17H17BN3+·I−·H2O, is a di­aza­borinane featuring substitution at the 1, 2, and 3 positions in the nitro­gen–boron six-membered heterocycle. The cation is approximately planar with a dihedral angle between the pyridyl ring and the di­aza­borinane ring system of 5.40 (5)°. In the crystal, the cations stack along [100] in an alternating head-to-tail manner, while the iodide ion and water mol­ecule form one-dimensional hydrogen-bonded chains beside the cation stack. The cation stacks and I−–water chains are crosslinked by N—H⋯I and N—H⋯O hydrogen bonds.




no

Chlorido­(2-{(2-hy­droxy­eth­yl)[tris­(hy­droxy­meth­yl)meth­yl]amino}­ethano­lato-κ5N,O,O',O'',O''')copper(II)

The title complex, [Cu(C8H18NO5)Cl] or [Cu(H4bis-tris­)Cl], was obtained starting from the previously reported [Cu(H5bis-tris­)Cl]Cl compound. The deprotonation of the amino­polyol ligand H5bis-tris {[bis­(2-hy­droxy­eth­yl)amino]­tris­(hy­droxy­meth­yl)methane, C8H19NO5} promotes the formation of a very strong O—H⋯O inter­molecular hydrogen bond, characterized by an H⋯O separation of 1.553 (19) Å and an O—H⋯O angle of 178 (4)°. The remaining hy­droxy groups are also engaged in hydrogen bonds, forming R22(8), R44(16), R44(20) and R44(22) ring motifs, which stabilize the triperiodic supra­molecular network.




no

Poly[[{μ2-5-[(di­methyl­amino)(thioxo)meth­oxy]benzene-1,3-di­carboxyl­ato-κ4O1,O1':O3,O3'}(μ2-4,4'-di­pyridyl­amine-κ2N4:N4')cobalt(II)] di­methyl­formamide hemisolvate monohydrate]

In the crystal structure of the title compound, {[Co(C11H9NSO5)(C10H9N3)]0.5C3H7NO·H2O}n or {[Co(dmtb)(dpa)]·0.5DMF·H2O}n (dmtb2– = 5-[(di­meth­yl­amino)­thioxometh­oxy]-1,3-benzene­dicarboxyl­ate and dpa = 4,4'-di­pyridyl­amine), an assembly of periodic [Co(C11H9NSO5)(C10H9N3)]n layers extending parallel to the bc plane is present. Each layer is constituted by distorted [CoO4N2] octa­hedra, which are connected through the μ2-coordination modes of both dmtb2– and dpa ligands. Occupationally disordered water and di­meth­yl­formamide (DMF) solvent mol­ecules are located in the voids of the network to which they are connected through hydrogen-bonding inter­actions.




no

2-Oxo-2H-chromen-4-yl 3,3-di­methyl­butano­ate

In the crystal of the title compound, C15H16O4, the mol­ecules are connected through C—H⋯O hydrogen bonds, generating [100] chains, which are crosslinked by weak π–π stacking inter­actions.




no

Chlorido­[5,10,15,20-tetra­kis­(quinoline-7-carboxamido)­porphinato]iron(III)

The title compound, [Fe(C84H52N12O4)Cl], crystallizes in space group C2/c. The central FeIII cation (site symmetry 2) is coordinated in a fivefold manner, with four pyrrole N atoms of the porphyrin core in the basal sites and one Cl atom (site symmetry 2) in the apical position, which completes a slightly distorted square-pyramidal environment. The porphyrin macrocycle shows a characteristic ruffled-shape distortion and the iron atom is displaced out of the porphyrin plane by 0.42 Å with the average Fe—N distance being 2.054 (4) Å; the Fe—Cl bond length is 2.2042 (7) Å. Inter­molecular C—H⋯N and C—H⋯O hydrogen bonds occur in the crystal structure.




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Triaceto­nitrile­(1,4,7-trimethyl-1,4,7-tri­aza­cyclonona­ne)cobalt(II) bis­(tetra­phenyl­borate)

The title cobalt(II) complex, [Co(C2H3N)3(C9H21N3)](C24H20B)2 or [(tacn)Co(NCMe)3][BPh4]2, has been characterized by single-crystal X-ray diffraction. It incorporates the well-known macrocyclic tacn (1,4,7-trimethyl-1,4,7-tri­aza­cyclo­nona­ne) ligand, which is coordinated facially to the metal center. The complex crystallizes in space group P21/c with Z = 4. The divalent cobalt ion exhibits a six-coordinate octa­hedral geometry by one tacn and three aceto­nitrile ligands. Two non-coordinating tetra­phenyl­borate (BPh4−) anions are also present.




no

Bis(8-hy­droxy­quinolinium) naphthalene-1,5-di­sulfonate tetra­hydrate

The inter­action between 8-hy­droxy­quinoline (8HQ, C9H7NO) and naphthalene-1,5-di­sulfonic acid (H2NDS, C10H8O6S2) in aqueous media results in the formation of the salt hydrate bis­(8-hy­droxy­quinolinium) naphthalene-1,5-di­sulfonate tetra­hydrate, 2C9H8NO+·C10H6O6S22−·4H2O. The asymmetric unit comprises one protonated 8HQ+ cation, half of an NDS2– dianion symmetrically disposed around a center of inversion, and two water mol­ecules. Within the crystal structure, these components are organized into chains along the [010] and [10overline{1}] directions through O—H⋯O and N—H⋯O hydrogen-bonding inter­actions, forming a di-periodic network parallel to (101). Additional stabilizing inter­actions such as C—H⋯O, C—H⋯π, and π–π inter­actions extend this arrangement into a tri-periodic network structure




no

Poly[[μ3-2-(benzotriazol-1-yl)acetato-κ3O:O':N3]chlorido­(ethanol-κO)cobalt(II)]

In the title compound, [Co(C8H6N3O2)Cl(C2H5OH)]n, the CoII atoms adopt octa­hedral trans-CoN2O4 and tetra­hedral CoCl2O2 coordination geometries (site symmetries overline{1} and m, respectively). The bridging μ3-O:O:N 2-(benzotriazol-1-yl)acetato ligands connect the octa­hedral cobalt nodes into (010) sheets and the CoCl2 fragments link the sheets into a tri-periodic network. The structure displays O—H⋯O hydrogen bonding and the ethanol mol­ecule is disordered over two orientations.




no

(η6-Benzene)­chlorido­[(S)-2-(4-isopropyl-4,5-di­hydro­oxazol-2-yl)phenolato]ruthenium(II)

The title compound, [Ru(C12H14NO2)Cl(η6-C6H6)], exhibits a half-sandwich tripod stand structure and crystallizes in the ortho­rhom­bic space group P212121. The arene group is η6 π-coordinated to the Ru atom with a centroid-to-metal distance of 1.6590 (5) Å, with the (S)-2-(4-isopropyl-4,5-di­hydro­oxazol-2-yl)phenolate chelate ligand forming a bite angle of 86.88 (19)° through its N and phenolate O atoms. The pseudo-octa­hedral geometry assumed by the complex is completed by a chloride ligand. The coordination of the optically pure bidentate ligand induces metal centered chirality onto the complex with a Flack parameter of −0.056.




no

4-[(2-Phenyl­eth­yl)amino]­benzoic acid

The title compound, C15H15NO2, crystallizes with two mol­ecules in the asymmetric unit. In the crystal, the two mol­ecules associate to form an acid–acid dimer by pairwise O—H⋯O hydrogen bonds.




no

Norfloxacinium nitrate

In the title salt [systematic name: 4-(3-carb­oxy-1-ethyl-6-fluoro-4-oxo-1,4-di­hydro­quin­olin-7-yl)piperazin-1-ium nitrate], C16H19FN3O3+·NO3−, proton transfer from nitric acid to the N atom of the piperazine ring of norfloxacin has occurred to form a mol­ecular salt. In the extended structure, N—H⋯O hydrogen bonds link alternating cations and anions into [100] chains, which are reinforced by aromatic π–π stacking inter­actions between the quinoline moieties of the norfloxacinium cations.




no

Bis(2-carb­oxy­quinolinium) hexa­chlorido­stan­nate(IV) dihydrate

In the hydrated title salt, (C10H8NO2)2[SnCl6]·2H2O, the tin(IV) atom is located about a center of inversion. In the crystal structure, the organic cation, the octa­hedral inorganic anion and the water mol­ecule of crystallization inter­act through O—H⋯O, N—H⋯O and O—H⋯Cl hydrogen bonds, supplemented by weak π–π stacking between neighboring cations, and C—Cl⋯π inter­actions.




no

Poly[tris­(2-amino­butan-1-ol)copper(II) [hexa­kis-μ2-cyanido-κ12C:N-tetra­copper(I)] bis­(2-amino­butan-1-olato)aqua­copper(II) monohydrate]

The title structure, {[Cu(C4H11NO)3][Cu4(CN)6]·[Cu(C4H10NO)2(H2O)]·H2O}n, is made up of diperiodic honeycomb CuICN networks built from [Cu4(CN)6]2− units, together with two independent CuII complexes: six-coord­inate [Cu(CH3CH2CH(NH2)CH2OH)3]2+ cations, and five-coordinate [Cu(CH3CH2CH(NH2)CH2O)2·H2O] neutral species. The two CuII complexes are not covalently bonded to the CuICN networks. Strong O—H⋯O hydrogen bonds link the CuII complexes into pairs and the pairs are hydrogen bonded into chains along the crystallographic b axis via the hydrate water mol­ecule. In addition, O—H⋯(CN) and N—H⋯(CN) hydrogen bonds link the cations to the CuCN network. In the honeycomb polymeric moiety, all bridging cyanido ligands are disordered over two orientations, head-to-tail and tail-to-head, with occupancies for C and N atoms varying for each CN group.




no

catena-Poly[[(8-amino­quinoline)­cobalt(II)]-di-μ-azido]

The title coordination polymer, [Co(N3)2(C9H8N2)]n, was synthesized solvothermally. The CoII atom exhibits a distorted octa­hedral [CoN6] coordination geometry with a bidentate 8-amino­quinoline ligand and four azide ligands. Bridging azide ligands result in chains extending along [100]. N—H⋯N hydrogen bonds join the chains to give an extended structure with sheets parallel to (002).




no

Bis[2-(isoquinolin-1-yl)phenyl-κ2N,C1](2-phenyl-1H-imidazo[4,5-f][1,10]phenanthroline-κ2N,N')iridium(III) hexa­fluorido­phosphate methanol monosolvate

The title compound, [Ir(C15H10N)2(C19H12N4)]PF6·CH3OH, crystallizes in the C2/c space group with one monocationic iridium complex, one hexa­fluorido­phosphate anion, and one methanol solvent mol­ecule of crystallization in the asymmetric unit, all in general positions. The anion and solvent are linked to the iridium complex cation via hydrogen bonding. All bond lengths and angles fall into expected ranges compared to similar compounds.




no

(1R,2S,4aR,6S,8R,8aS)-1-(3-Hy­droxy­propano­yl)-1,3,6,8-tetra­methyl-1,2,4a,5,6,7,8,8a-octa­hydronaphthalene-2-carb­oxy­lic acid

The mol­ecular structure of C18H28O4, (+)-diplodiatoxin, is described, whereby the absolute configuration of the structure of diplodiatoxin has been confirmed by single-crystal X-ray diffraction. Diplodiatoxin crystallizes in the chiral P43212 space group with one mol­ecule in the asymmetric unit.




no

Δ-Bis[(S)-2-(4-isopropyl-4,5-di­hydro­oxazol-2-yl)phenolato-κ2N,O1](1,10-phenanthroline-κ2N,N')ruthenium(III) hexa­fluorido­phosphate

The title compound, [Ru(C12H14NO2)2(C12H8N2)]PF6 crystallizes in the tetra­gonal Sohnke space group P41212. The two bidentate chiral salicyloxazoline ligands and the phenanthroline co-ligand coordinate to the central RuIII atom through N,O and N,N atom pairs to form bite angles of 89.76 (15) and 79.0 (2)°, respectively. The octa­hedral coordination of the bidentate ligands leads to a propeller-like shape, which induces metal-centered chirality onto the complex, with a right-handed (Δ) absolute configuration [the Flack parameter value is −0.003 (14)]. Both the complex cation and the disordered PF6− counter-anion are located on twofold rotation axes. Apart from Coulombic forces, the crystal cohesion is ensured by non-classical C—H⋯O and C—H⋯F inter­actions.




no

(Z)-N-(2,6-Diiso­propyl­phen­yl)-1-[(2-meth­oxyphen­yl)amino]­methanimine oxide

The mol­ecular structure of the title compound, C20H26N2O2 reveals non-co-planarity between the central formamidine backbone and each of the outer meth­oxy- and i-propyl- substituted benzene rings with dihedral angles of 7.88 (15) and 81.17 (15)°, respectively, indicating significant twists in the mol­ecule. In the crystal, inter­molecular C—H⋯O inter­actions, forming an R34(30) graph set, occur within a two-dimensional layer that extends along the ac plane.




no

(Z)-N-(2,6-Di­methyl­phen­yl)-1-[(2-meth­oxy­phen­yl)amino]­methanimine oxide methanol monosolvate

In the title solvate, C16H18N2O2·CH4O, the dihedral angles between the formamidine backbone and the pendant 2-meth­oxy­phenyl and 2,6-di­methyl­phenyl groups are 14.84 (11) and 81.61 (12)°, respectively. In the crystal, the components are linked by C—H⋯O, O—H⋯O and C—H⋯ π hydrogen bonds, generating a supra­molecular chain that extends along the crystallographic a-axis direction.