Search

K-feldspar represents an important natural resource of potassium and aluminum. Within the framework of this study, the K-feldspar was mechanically activated in a planetary ball mill under different conditions planned according to 43 Taguchi orthogonal array experimental design. As outputs, specific surface area (SBET), median particle size (d50), amorphization degree of mineral phases , and Al recovery were used. It was found that the initial d50 value of 293 μm could be reduced to 6.7 μm and the SBET value of 4.7 m2/g could be increased up to 32.5 m2/g upon milling. Both microcline KAl3SiO8, and albite NaAl3SiO8 could be almost completely amorphized, whereas quartz SiO2 still maintained some crystallinity even under the most intensive conditions. Increasing SBET and decreasing the d50 values did not lead to a significant improvement in Al leach recovery, whereas a clear relationship between the amorphization of microcline and the recovered aluminum was found. Analysis of Variance (ANOVA) showed that increasing ball-to-powder ratio is the most beneficial for the improvement in Al recovery. In situ powder X-ray diffraction monitoring performed in an oscillation ball mill under synchrotron irradiation has shown very rapid amorphization of microcline phase at the beginning. However, amorphization of microcline was only partial after two hours of the treatment in this mill, apart from almost complete process in the planetary ball mill. In the end, regressions for the calculation of Al recovery by knowing the values of input parameters were calculated. In general, by just using mechanical activation without the subsequent roasting process that is commonly used to boost metal recoveries, it was possible to quantitatively recover aluminum from K-feldspar.

In materials science, traditional techniques for analyzing layered structures are essential for obtaining information about local structure, electronic properties and chemical states. While valuable, these methods often require high vacuum environments and have limited depth profiling capabilities. The grazing exit x-ray absorption near-edge structure (GE-XANES) technique addresses these limitations by providing depth-resolved insight at ambient conditions, facilitating in situ material analysis without special sample preparation. However, GE-XANES is limited by long data acquisition times, which hinders its practicality for various applications. To overcome this, we have incorporated Bayesian optimization (BO) into the GE-XANES data acquisition process. This innovative approach potentially reduces measurement time by a factor of 50. We have used a standard GE-XANES experiment, which serve as reference, to validate the effectiveness and accuracy of the BO-informed experimental setup. Our results show that this optimized approach maintains data quality while significantly improving efficiency, making GE-XANES more accessible to a wider range of materials science applications.

Abstract Metal nanoparticles have a substantial impact across different fields of science, such as photochemistry, energy conversion, and medicine. Among the commonly used nanoparticles, silver nanoparticles are of special interest due to their antibacterial properties and applications in sensing and catalysis. However, many of the methods used to synthesize silver nanoparticles often do not result in well-defined products, the main obstacles being high polydispersity or a lack of particle size tunability. We describe an automated approach to on-demand synthesis of adjustable particles with mean radii of 3 and 5 nm using the polyol route. The polyol process is a promising route for silver nanoparticles e.g., to be used as reference materials. We characterised the as-synthesized nanoparticles using small-angle X-ray scattering, dynamic light scattering and further methods, showing that automated synthesis can yield colloids with reproducible and tuneable properties.

Human-robot interaction research has shown that social robots can interact with humans in complex social situations and display leadership-related behaviors. Therefore, social robots could be able to take on leadership roles. The aim of our study was to investigate human followers’ perceptions and reactions towards robot leadership behavior, and differences based on the robot’s displayed leadership style. We implemented a robot to show either a transformational or a transactional leadership style in its speech and its movements. We presented the robot to university and executive MBA students (N = 29) and subsequently conducted semi-structured interviews and group discussions. The results of explorative coding indicated that participants differed in their perceptions and reactions based on the robot’s leadership style and based on their assumptions about robots in general. We observed that participants quickly imagined either a utopia or worried about a dystopia, depending on the robot’s leadership style and their assumptions, and that a subsequent reflection led to more nuanced views. We discuss the implications and recommendations for human-robot interaction and leadership research.

Recruitment contexts such as STEM professorships promote clearly defined selection criteria and objective assessment. We illuminate in these contexts, the subjective interpretation of seemingly objective criteria and gendered arguments in discussions of applicants. Additionally, we explore gender bias despite comparable applicant profiles investigating how specific success factors lead to selection recommendations for male and female applicants. Implementing a mixed methods approach, we aim to highlight the influence of heuristics, stereotyping, and signaling in applicant assessments. We interviewed 45 STEM professors. They answered qualitative open-ended interview questions, and evaluated hypothetical applicant profiles, qualitatively and quantitatively. The applicant profiles enabled a conjoint experiment with different applicant attributes varied across the profiles (i.e., publications, willingness to cooperate, network recommendation, and applicant gender), the interviewees indicating scores of selection recommendation while thinking aloud. Our findings reveal gendered arguments, i.e., questioning women potentially fueled by a perception of women’s exceptional status and perceived self-questioning of women. Furthermore, they point to gender-independent and gender-dependent success patterns, thereby to potential success factors particularly for female applicants. We contextualize and interpret our quantitative findings in light of professors’ qualitative statements.

Time-resolved in situ (TRIS) X-ray powder diffraction promises great potential to study mechanochemical processes. Here, the authors develop a strategy to enhance the resolution of TRIS experiments to allow deeper interpretation of mechanochemical transformations; the method is applied to a variety of model systems including inorganic, metal-organic, and organic mechanosyntheses.

Mechanically flexible single crystals are promising materials for advanced technological applications. Here, the authors study the high pressure response of a plastically flexible coordination polymer and provide indication of an overall disparate mechanical response of bulk flexibility and quasi-hydrostatic compression within the same crystal lattice.

Catalysts derived from pyrolysis of metal organic frameworks (MOFs) are promising candidates to replace expensive and scarce platinum-based electrocatalysts commonly used in polymer electrolyte membrane fuel cells. MOFs contain ordered connections between metal centers and organic ligands. They can be pyrolyzed into metal- and nitrogen-doped carbons, which show electrocatalytic activity toward the oxygen reduction reaction (ORR). Furthermore, metal-free heteroatom-doped carbons, such as N-F-Cs, are known for being active as well. Thus, a carbon material with Co-N-F doping could possibly be even more promising as ORR electrocatalyst. Herein, we report the mechanochemical synthesis of two polymorphs of a zeolitic imidazole framework, Co-doped zinc 2-trifluoromethyl-1H-imidazolate (Zn0.9Co0.1(CF3-Im)2). Time-resolved in situ X-ray diffraction studies of the mechanochemical formation revealed a direct conversion of starting materials to the products. Both polymorphs of Zn0.9Co0.1(CF3-Im)2 were pyrolyzed, yielding Co-N-F containing carbons, which are active toward electrochemical ORR.

While some individuals tend to follow norms, others, in the face of tempting but forbidden options, tend to commit rule-breaking when this action is beneficial for themselves. Previous studies have neglected such interindividual differences in rule-breaking. The present study fills this gap by investigating cognitive characteristics of individuals who commit spontaneous deliberative rule-breaking (rule-breakers) versus rule-followers. We developed a computerised task, in which 133 participants were incentivised to sometimes violate set rules which would-if followed-lead to a loss. While 52% of participants tended to break rules to obtain a benefit, 48% tended to follow rules even if this behaviour led to loss. Although rule-breakers experienced significantly more cognitive conflict (measured via response times and mouse movement trajectories) than rule-followers, they also obtained higher payoffs. In rule-breakers, cognitive conflict was more pronounced when violating the rules than when following them, and mainly during action planning. This conflict increased with frequent, recurrent, and early rule-breaking. Our results were in line with the Decision-Implementation-Mandatory switch-Inhibition model and thus extend the application of this model to the interindividual differences in rule-breaking. Furthermore, personality traits such as extroversion, disagreeableness, risk propensity, high impulsiveness seem to play a role in the appreciation of behaviours and cognitive characteristics of rule-followers and rule-breakers. This study opens the path towards the understanding of the cognitive characteristics of the interindividual differences in responses towards rules, and especially in spontaneous deliberative rule-breaking.

The transformation of a base-catalyzed, mechano-assisted Knoevenagel condensation of mono-fluorinated benzaldehyde derivatives (p-, m-, o-benzaldehyde) with malonodinitrile was investigated in situ and in real time. Upon milling, the para-substituted product was found to crystallize initially into two different polymorphic forms, depending on the quantity of catalyst used. For low catalyst concentrations, a mechanically metastable phase (monoclinic) was initially formed, converting to the mechanically stable phase (triclinic) upon further grinding. Instead, higher catalyst concentrations crystallize directly as the triclinic product. Inclusion of catalyst in the final product, as evidenced by mass spectrometric analysis, suggests this complex polymorphic pathway may be due to seeding effects. Multivariate analysis for the in situ Raman spectra supports this complex formation pathway, and offers a new approach to monitoring multi-phase reactions during ball milling.

Over the decades, the application of mechanical force to influence chemical reactions has been called by various names: mechanochemistry, tribochemistry, mechanical alloying, to name but a few. The evolution of these terms has largely mirrored the understanding of the field. But what is meant by these terms, why have they evolved, and does it really matter how a process is called? Which parameters should be defined to describe unambiguously the experimental conditions such that others can reproduce the results, or to allow a meaningful comparison between processes explored under different conditions? Can the information on the process be encoded in a clear, concise, and self-explanatory way? We address these questions in this Opinion contribution, which we hope will spark timely and constructive discussion across the international mechanochemical community.

The proneness to be sexually aroused, to perform sexual acts, or to be sexually disinhibited during a particular mood varies across individuals. However, the physiological mechanisms underlying this specific and variable relationship between mood and sex-related processes are poorly understood. We propose that cortisol may act as an important moderator in this as it has shown to influence sexual arousal and to play a neuromodulatory role during emotion regulation. Here, we conducted a functional magnetic resonance imaging study in a sample of young males to investigate whether cortisol modulates the neural response during the approach of sexual stimuli in an approach-avoidance task and whether this potential relationship explains the individual differences in sexual inhibition and in mood-related sexual interest and activity. We revealed that cortisol associates with the anteromedial prefrontal cortex activation during the approach towards sexual stimuli. Moreover, this anteromedial prefrontal cortex response was dependent on individual differences in sexual inhibition and the improvements of negative mood as a result of sexual activity. The anteromedial prefrontal cortex is already known to process bottom-up information, reward, and risk estimation. The neuromodulatory role of cortisol within this region during sexual approach may represent a previously unknown yet key element in the regulation of sexual behavior in young males.

Abstract Decisions are often governed by rules on adequate social behaviour. Recent research suggests that the right lateral prefrontal cortex (rLPFC) is involved in the implementation of internal fairness rules (norms), by controlling the impulse to act selfishly. A drawback of these studies is that the assumed norms and impulses have to be deduced from behaviour and that norm-following and pro-sociality are indistinguishable. Here, we directly confronted participants with a rule that demanded to make advantageous or disadvantageous monetary allocations for themselves or another person. To disentangle its functional role in rule-following and pro-sociality, we divergently manipulated the rLPFC by applying cathodal or anodal transcranial direct current stimulation (tDCS). Cathodal tDCS increased participants’ rule-following, even of rules that demanded to lose money or hurt another person financially. In contrast, anodal tDCS led participants to specifically violate more often those rules that were at odds with what participants chose freely. Brain stimulation over the rLPFC thus did not simply increase or decrease selfishness. Instead, by disentangling rule-following and pro-sociality, our results point to a broader role of the rLPFC in integrating the costs and benefits of rules in order to align decisions with internal goals, ultimately enabling to flexibly adapt social behaviour.

Organic single crystals that combine mechanical flexibility and optical properties are important for developing flexible optical devices, but examples of such crystals remain scarce. Both mechanical flexibility and optical activity depend on the underlying crystal packing and the nature of the intermolecular interactions present in the solid state. Hence, both properties can be expected to be tunable by small chemical modifications to the organic molecule. By incorporating a chlorine atom, a reportedly mechanically flexible crystal of (E)-1-(4-bromo-phenyl)iminomethyl-2-hydroxyl-naphthalene (BPIN) produces (E)-1-(4-bromo-2-chloro-phenyl)iminomethyl-2-hydroxyl-naphthalene (BCPIN). BCPIN crystals show elastic bending similar to BPIN upon mechanical stress, but exhibit a remarkable difference in their optical properties as a result of the chemical modification to the backbone of the organic molecule. This work thus demonstrates that the optical properties and mechanical flexibility of molecular materials can, in principle, be tuned independently.

The mechanochemical Knoevenagel condensation of malononitrile with p-nitrobenzaldehyde was studied in situ using a tandem approach. X-ray diffraction and Raman spectroscopy were combined to yield time-resolved information on the milling process. Under solvent-free conditions, the reaction leads to a quantitative conversion to p-nitrobenzylidenemalononitrile within 50 minutes. The in situ data indicate that the process is fast and proceeds under a direct conversion. After stopping the milling process, the reaction continues until complete conversion. The continuous and the stopped milling process both result in crystalline products suitable for single crystal X-ray diffraction.

The growing sense of insecurity in the Western world due to home-grown Islamist terrorism prompts further research on the topic. Based on previous literature, the current paper attempts to determine whether factors can be identified which contribute to Western individuals joining Islamic extremist organizations and engaging in terrorist behavior in the West. Four factors are discussed: While extensive scientific literature supports the view that identity crises and relative deprivation play a crucial role in turning Western individuals to terrorism, evidence on the role of personal characteristics and empathy, on the other hand, is still too scarce to allow any clear scientific judgment.

Metal-organic frameworks (MOFs) are promising nanoporous materials with many practical applications. This owes largely to their remarkable porosity and the presence of specific chemical functionalities, such as exposed metal sites (EMS). The MOF-74 structure is known for exhibiting one of the highest EMS densities among porous materials. Moreover, the inclusion of structural defects has been proposed to enhance activity further. This was previously achieved by mixing the original linker together with a second one, having lower topology. The presence of structural defects was evidenced by the resulting crystalline properties and thermal stability. In this work, different mixtures of tetratopic 2,5-dihydroxyterephthalic acid with up to 60% of the tritopic hydroxyterephtalic acid were used to synthesize crystalline Co-MOF-74-like materials. Materials synthesized from higher proportions than 30% of hydroxyterephtalic acid in the synthesis media collapse upon partial removal of the solvent molecules. This indicates the presence of structural defects and the importance of the solvent molecules in stabilizing the crystalline structures. Electron microscope images show that crystal size reduces with inclusion of hydroxyterephtalic acid as the second linker. The presence of coordinated solvent molecules at the EMS was evaluated by Fourier-transform infrared spectra (FTIR) spectroscopy, so that a higher degree of solvent-exchange was observed during washing for defective structures. Furthermore, TG analysis suggests defective structures exhibit lower desolvation temperatures than the defect-free structures. Finally, N2 adsorption-desorption analyses at −196°C showed an enhanced accessibility of the gas to the inner porosity of the defective structures and therefore, the EMS of the material. All these finding make this pathway interesting to enhance the potential interest of these materials for an industrial application because of both a facilitated activation and a better access to the active sites.

The successful inhibition of sexual thoughts, desires, and behaviors represents an essential ability for adequate functioning in our daily life. Evidence derived from lesion studies indicates a link between sexual inhibition and the general ability for behavioral and cognitive control. This is further supported by the high comorbidity of sexual compulsivity with other inhibition-related disorders. Here, we aimed at investigating whether sexual and general inhibition recruit overlapping or distinct neural correlates in the brain. Furthermore, we investigated the specificity of two different kinds of sexual inhibition: inhibition of sexually driven motor responses and inhibition of sexual incoming information. To this end, 22 healthy participants underwent functional Magnetic Resonance Imaging (fMRI) while performing a task requiring general response inhibition (Go/No-go), as well as cognitive and motivational sexual inhibition (Negative Affective Priming and Approach-Avoidance task). Our within-subject within-session design enabled the direct statistical comparison between general and sexual inhibitory mechanisms. The general inhibition task recruited mainly prefrontal and insular regions, replicating previous findings. In contrast, the two types of sexual inhibition activated both common and distinct neural networks. Whereas cognitive sexual inhibition engaged the inferior frontal gyrus, the orbitofrontal cortex and the fusiform gyrus, motivational sexual inhibition was characterized by a hypoactivation in the anterolateral prefrontal cortex. Both types of sexual inhibition recruited the inferior frontal gyrus and the inferotemporal cortex. However, the activity of the inferior frontal gyrus did not correlate with behavioral inhibitory scores. These results support the hypothesis of inhibitory processing being an emergent property of a functional network.

The choice of solvents influences crystalline solid formed during the crystallization of active pharmaceutical ingredients (API). The underlying effects are not always well understood because of the complexity of the systems. Theoretical models are often insufficient to describe this phenomenon. In this study, the crystallization behavior of the model drug paracetamol in different solvents was studied based on experimental and molecular dynamics data. The crystallization process was followed in situ using time-resolved Raman spectroscopy. Molecular dynamics with simulated annealing algorithm was used for an atomistic understanding of the underlying processes. The experimental and theoretical data indicate that paracetamol molecules adopt a particular geometry in a given solvent predefining the crystallization of certain polymorphs.

Tuning and controlling the solid-state photophysical properties of organic luminophore are very important to develop next-generation organic luminescent materials. With the aim of discovering new functional luminescent materials, new cocrystals of 9-anthracene carboxylic acid (ACA) were prepared with two different dipyridine coformers: 1,2-bis(4-pyridyl)ethylene and 1,2-bis(4-pyridyl)ethane. The cocrystals were successfully obtained by both mechanochemical approaches and conventional solvent crystallization. The newly obtained crystalline solids were characterized thoroughly using a combination of single crystal X-ray diffraction, powder X-ray diffraction, Fourier-transform infrared spectroscopy, differential thermal analysis, and thermogravimetric analysis. Structural analysis revealed that the cocrystals are isostructural, exhibiting two-fold interpenetrated hydrogen bonded networks. While the O–H···N hydrogen bonds adopts a primary role in the stabilization of the cocrystal phases, the C–H···O hydrogen bonding interactions appear to play a significant role in guiding the three-dimensional assembly. Both π···π and C–H···π interactions assist in stabilizing the interpenetrated structure. The photoluminescence properties of both the starting materials and cocrystals were examined in their solid states. All the cocrystals display tunable photophysical properties as compared to pure ACA. Density functional theory simulations suggest that the modified optical properties result from charge transfers between the ACA and coformer molecules in each case. This study demonstrates the potential of crystal engineering to design solid-state luminescence switching materials through cocrystallization.

Nickel nanoparticles are an active research area due to their multiple applications as catalysts in different processes. A variety of preparation techniques have been reported for the synthesis of these nanoparticles, including solvothermal, microwave-assisted, and emulsion techniques. The well-studied solvothermal oleylamine synthesis route comes with the drawback of needing standard air-free techniques and often space-consuming glassware. Here, we present a facile and straightforward synthesis method for size-controlled highly monodisperse nickel nanoparticles avoiding the use of, e.g., Schlenk techniques and space-consuming labware. The nanoparticles produced by this novel synthetic route were investigated using small-angle X-ray scattering, transmission electron microscopy, X-ray diffraction, and X-ray spectroscopy. The nanoparticles were in a size range of 4–16 nm, show high sphericity, no oxidation, and no agglomeration after synthesis.

Cognitive effort and self-control are exhausting. Although evidence is ambiguous, behavioural studies have repeatedly suggested that control-demanding tasks seem to deplete a limited cache of self-regulatory resources leading to performance degradations and fatigue. While resource depletion has indirectly been associated with a decline in right prefrontal cortex capacity, its precise neural underpinnings have not yet been revealed. This study consisted of two independent experiments, which set out to investigate the causal role of the right dorsolateral prefrontal cortex (DLPFC) in a classic dual phase depletion paradigm employing non-invasive brain stimulation. In Experiment 1 we demonstrated a general depletion effect, which was significantly eliminated by anodal transcranial Direct Current Stimulation to the right DLPFC. In Experiment 2, however, we failed to replicate the basic psychological depletion effect within a second independent sample. The dissimilar results are discussed in the context of the current 'replication crisis' and suggestions for future studies are offered. While our current results do not allow us to firmly argue for or against the existence of resource depletion, we outline why it is crucial to further clarify which specific external and internal circumstances lead to limited replicability of the described effect. We showcase and discuss the current inter-lab replication problem based on two independent samples tested within one research group (intra-lab).

The preparation of new active pharmaceutical ingredient (API) multicomponent crystal forms, especially co-crystals and salts, is being considered as a reliable strategy to improve API solubility and bioavailability. In this study, three novel imidazole-based salts of the poorly water-soluble salicylic acid (SA) are reported exhibiting a remarkable improvement in solubility and dissolution rate properties. All structures were solved by powder X-ray diffraction. Multiple complementary techniques were used to solve co-crystal/salt ambiguities: density functional theory calculations, Raman and 1H/13C solid-state NMR spectroscopies. In all molecular salts, the crystal packing interactions are based on a common charged assisted +N-H(SA) ⋯ O−(co-former) hydrogen bond interaction. The presence of an extra methyl group in different positions of the co-former, induced different supramolecular arrangements, yielding salts with different physicochemical properties. All salts present much higher solubility and dissolution rate than pure SA. The most promising results were obtained for the salts with imidazole and 1-methylimidazole co-formers.

In September 2018, the First European Workshop on Metal Phosphonates Chemistry brought together some prominent researchers in the field of metal phosphonates and phosphinates with the aim of discussing past and current research efforts and identifying future directions. The scope of this perspective article is to provide a critical overview of the topics discussed during the workshop, which are divided into two main areas: synthesis and characterisation, and applications. In terms of synthetic methods, there has been a push towards cleaner and more efficient approaches. This has led to the introduction of high-throughput synthesis and mechanochemical synthesis. The recent success of metal−organic frameworks has also promoted renewed interest in the synthesis of porous metal phosphonates and phosphinates. Regarding characterisation, the main advances are the development of electron diffraction as a tool for crystal structure determination and the deployment of in situ characterisation techniques, which have allowed for a better understanding of reaction pathways. In terms of applications, metal phosphonates have been found to be suitable materials for several purposes: they have been employed as heterogeneous catalysts for the synthesis of fine chemicals, as solid sorbents for gas separation, notably CO2 capture, as materials for electrochemical devices, such as fuel cells and rechargeable batteries, and as matrices for drug delivery.

The insular cortex has consistently been associated with various aspects of emotion regulation and social interaction, including anger processing and overt aggression. Aggression research distinguishes proactive or instrumental aggression from retaliation, i.e. aggression in response to provocation. Here, we investigated the specific role of the insular cortex during retaliation, employing a controlled behavioral aggression paradigm implementing different levels of provocation. Fifteen healthy male volunteers underwent whole brain functional magnetic resonance imaging (fMRI) to identify brain regions involved in interaction with either a provoking or a non-provoking opponent. FMRI group analyses were complemented by examining the parametric modulations of brain activity related to the individual level of displayed aggression. These analyses identified a hemispheric lateralization as well as an anatomical segregation of insular cortex with specifically the left posterior part being involved in retaliation. The left-lateralization of insular activity during retaliation is in accordance with evidence from electro-physiological studies, suggesting left-lateralized fronto-cortical dominance during anger processing and aggressive acts. The posterior localization of insular activity, on the other hand, suggests a spatial segregation within insular cortex with particularly the posterior part being involved in the processing of emotions that trigger intense bodily sensations and immediate action tendencies.

The title compound, C18H25BrO, crystallized as a racemate with four independent molecules in the asymmetric unit. In the crystal, three of these four molecules are linked via C—Br...Br—C halogen bonds [Br...Br = 3.662 (2) and 3.652 (2) Å], forming dimers.

The title compound, {2-[(2-carbamoylethyl)amino]-3-methylpentanoic acid}, C9H18N2O3, is of interest with respect to its biological activity. It was formed during an addition reaction between acrylamide and the amino acid isoleucine. The crystal structure is a three-dimensional network built up by intermolecular N—H...O and O—H...N hydrogen bonds.

The title compound, C17H26O10, was formed by a Koenigs–Knorr reaction of 2,3,4,6-tetra-O-acetyl-α-d-glucopyranosyl bromide and propan-2-ol. The central ring adopts a chair conformation. The crystal does not contain any significant intermolecular interactions.

The racemic title compound, C3H5Br2NO, was crystallized from methanol. In the crystal, adjacent molecules are linked through N—H...O hydrogen bonds, forming chains along the c-axis direction. These chains are linked through N—H...O hydrogen bonds, forming an undulating two-dimensional network lying parallel to the bc plane. There are also short Br...Br contacts present [3.514 (3) Å].

The title compound [systematic name: (2R,3R,4S,5R,6R)-2-(acetoxymethyl)-6-propoxytetrahydro-2H-pyran-3,4,5-triyl triacetate], C17H26O10, was formed by a Koenigs–Knorr reaction of 2,3,4,6-tetra-O-acetyl-α-d-glucopyranosyl bromide and n-propanol. The central ring adopts a chair conformation. The crystal does not contain any significant interactions such as hydrogen bonds.

A new cocrystal of pyrazinamide with oxalic acid was prepared mechanochemically and characterized by PXRD, Raman spectroscopy, solid-state NMR spectroscopy, DTA-TG, and SEM. Based on powder X-ray diffraction data the structure was solved. The formation pathway of the reaction was studied in situ using combined synchrotron PXRD and Raman spectroscopy. Using oxalic acid dihydrate the initially neat grinding turned into a rapid self-accelerated liquid-assisted grinding process by the release of crystallization water. Under these conditions, the cocrystal was formed directly within two minutes.

In the crystal structure of the title compound, C8H10BrN2O+·Br−, intermolecular N—H...Br hydrogen bonds link the molecules into infinite chains along [001]. The inclined angle between the pyridine ring plane and the plane defined by the acid amide group is 63.97 (4)°.

The absolute configuration of the title compound, C18H24O5·H2O, was not been determined by anomalous-dispersion effects, but has been assigned by reference to an unchanging chiral centre in the synthetic procedure. Intramolecular O—H...O hydrogen bonds stabilize the molecular conformation. In the crystal, O—H...O hydrogen bonds link the main molecules and the water molecules, forming an infinite three-dimensional network.

The title compound {systematic name: (6aR,9S)-N-[(2R,5S,10aS,10bS)-5-benzyl-10b-hydroxy-2-methyl-3,6-dioxooctahydro-8H-oxazolo[3,2-a]pyrrolo[2,1-c]pyrazin-2-yl]-7-methyl-4,6,6a,7,8,9-hexahydroindolo[4,3-fg]quinoline-9-carboxamide}, C33H35N5O5, was formed by an epimerization reaction of ergotamine. The non-aromatic ring (ring C of the ergoline skeleton) directly fused to the aromatic rings is nearly planar [maximum deviation = 0.317 (4) Å] and shows an envelope conformation, whereas ring D, involved in an intramolecular N—H...N hydrogen bond exhibits a slightly distorted chair conformation. The structure displays chains running approximately parallel to the diagonal of bc plane that are formed through N—H...O hydrogen bonds.

The title compound, also known as cis-zearalenone (cis-ZEN), C18H22O5, has already been reported elsewhere [Griffin et al. (1981). ACA Ser. 29, 35], but no atomic coordinates are publicly available. The molecule is of interest with respect to its toxicity. In the crystal, intramolecular O—H...O hydrogen bonds stabilize the molecular conformation, while intermolecular O—H...O hydrogen bonds link the molecules to form infinite chains along the [110] and [1-10] directions. The absolute configuration has been assigned by reference to an unchanging chiral centre in the synthetic procedure.

In the title compound [systematic name: (7-methyl-4,6,6a,7,8,9-hexahydroindolo[4,3,2-fg]quinoline-9-yl)methanol monohydrate], C16H18N2O·H2O, the non-aromatic ring (ring C of the ergoline skeleton) directly fused to the aromatic rings is nearly planar, with a maximum deviation of 0.659 (3) Å, and shows an envelope conformation. In the crystal, hydrogen bonds between the lysergol and water molecules contribute to the formation of layers parallel to (10-2).

Crystals of the title compound, C18H26O2, were grown from ethyl acetate. Due to the racemic precursor, the title compound is also obtained as a racemate. Disorder was observed during structure refinement, originating from two possible half-chair conformations of the non-aromatic ring. The disorder was refined by introducing split positions in the cyclo-hexane ring regarding the two possible R and S-enantiomers at the chiral CH group [ratio 0.744 (3):0.256 (3)]. The crystal structure features pairs of inversion-related molecules connected by pairs of non-classical C—H...O hydrogen bonds.

In the title compound, C8H12Br4, the cyclohexane ring exhibits a chair conformation. The C—Br distances range from 1.964 (6) to 1.985 (5) Å and the C—C distances range from 1.496 (6) to 1.543 (7) Å. Short intermolecular Br...Br contacts [3.467 (4) Å] occur in the crystal.

The absolute configuration of ergometrinine, C19H23N3O2 {systematic name: (6aR,9S)-N-[(S)-1-hydroxypropan-2-yl]-7-methyl-4,6,6a,7,8,9-hexahydroindolo[4,3-fg]quinoline-9-carboxamide}, was established based on epimerization reaction of ergometrine, which was followed by preparative HPLC. The non-aromatic ring (ring C of the ergoline skeleton) directly fused to the aromatic rings is nearly planar [maximum deviation = 0.271 (3) Å] and shows an envelope conformation, whereas ring D, involved in an intramolecular N—H...N hydrogen bond, exibits a slightly distorted chair conformation. The structure displays undulating layers in the ac plane formed by O—H...O and N—H...O hydrogen bonds.

In the title compound (systematic name: 3,7,9-trihydroxy-1-methyl-6H-benzo[c]chromen-6-one), C14H10O5, the methyl group is shifted out of the molecular plane due to a steric collision, thus causing a slight twist of the benzene rings. The molecular structure is stabilized by an intramolecular O—H...O hydrogen bond, generating an S(6) ring. In the crystal, molecules are connected by intermolecular O—H...O hydrogen bonds into a three-dimensional network.

The title compound {systematic name: 4-methyl-N′-[(3E)-2-(1-methylpropyl)-5-oxopyrrolidin-3-ylidene]benzenesulfonohydrazide}, C15H21N3O3S, is the condensation product of deacetyl tenuazonic acid (DTA) and p-toluenesulfonohydrazide. The crystal structure consists of chains along [100] linked by N—H...O hydrogen bonds.

The heterocycle in the title compound {systematic name: (5S)-5-[(1S)-1-methylpropyl]pyrrolidine-2,4-dione}, C8H13NO2, is planar (r.m.s. deviation for all non-H atoms = 0.008 Å). The crystal structure is stabilized by N—H...O hydrogen bonding.

In the title compound, C16H19N5O6, two intramolecular N—H...O hydrogen bonds help to establish the conformation. In the crystal, intermolecular N—H...O links result in chains propagating in [010].

The hydrochloride salt of chiral l-nebivolol {systematic name: (+)−(R,S,S,S)-bis[2-(6-fluoro-3,4-dihydro-2H-1-benzopyran-2-yl)-2-hydroxyethyl]ammonium chloride dihydrate}, C22H26F2NO4+·Cl−·2H2O, was obtained by chiral liquid chromatography as a dihydrate. The pyran rings adopt half-chair conformations. Hydrogen bonds between the cation, anions and water molecules contribute to the formation of layers parallel to the ac plane.