Bridging the information gap in organic chemical reactions.

The varying quality of scientific reports is a well-recognized problem and often results from a lack of standardization and transparency in scientific publications. This situation ultimately leads to prominent complications such as reproducibility issues and the slow uptake of newly developed synthetic methods for pharmaceutical and agrochemical applications. In recent years, various impactful approaches have been advocated to bridge information gaps and to improve the quality of experimental protocols in synthetic organic publications.

Highly reflective Ru/Y multilayer mirrors for the spectral range of 9-11 nm.

The results of the investigation of the reflective characteristics of multilayer mirrors based on Ru/Y are presented. Reflection coefficients at the level of 38.5% at an operating wavelength of 9.

Chromium/Photoredox Dual Catalyzed Synthesis of α-Benzylic Alcohols, Isochromanones, 1,2-Oxy Alcohols and 1,2-Thio Alcohols.

Herein, a Cr/Photoredox-catalyzed general synthetic strategy to access α-benzylic alcohols, isochromanones, oxy alcohols and thio alcohols is unveiled. Alkylation of aldehydes being a crucial C-C bond forming reaction, designing competent catalytic systems would render an attractive and decorated set of diverse alcohol motifs. Considering the challenges associated with classical organometallic chemistry, the strategy of dual catalysis is applied here to generate diverse alcohol motifs in a mild and efficient manner.

Gadolinium Photocatalysis: Dearomative [2+2] Cycloaddition/Ring-Expansion Sequence with Indoles.

Lanthanide photocatalysts are much less investigated in synthetic chemistry than rare and expensive late transition metals. We herein introduce Gd photocatalysis of a highly regioselective, intermolecular [2+2] photocycloaddition/ring-expansion sequence with indoles, which could provide divergent access to cyclopenta[b]indoles and indolines. A simple and commercially available Gd(OTf) salt is sufficient for this visible-violet-light-induced transformation.

Optical constants of sputtered beryllium thin films determined from photoabsorption measurements in the spectral range 20.4-250 eV.

In this work, the refractive index of beryllium in the photon energy range 20.4-250 eV was experimentally determined. The initial data include measurements of the transmittance of two free-standing Be films with thicknesses of 70 nm and 152 nm, as well as reflectometric measurements of similar films on a substrate.

Soft X-ray varied-line-spacing gratings fabricated by near-field holography using an electron beam lithography-written phase mask.

A fabrication method comprising near-field holography (NFH) with an electron beam lithography (EBL)-written phase mask was developed to fabricate soft X-ray varied-line-spacing gratings (VLSGs). An EBL-written phase mask with an area of 52 mm × 30 mm and a central line density greater than 3000 lines mm was used. The introduction of the EBL-written phase mask substantially simplified the NFH optics for pattern transfer.

Optimized highly efficient multilayer-coated blazed gratings for the tender X-ray region.

The optimized design of multilayer-coated blazed gratings (MLBG) for high-flux tender X-ray monochromators was systematically studied by numerical simulations. The resulting correlation between the multilayer d-spacing and grating blaze angle significantly deviated from the one predicted by conventional equations. Three high line density gratings with different blaze angles were fabricated and coated by the same Cr/C multilayer.

Rapid Assessment of the Reaction-Condition-Based Sensitivity of Chemical Transformations.

A systematic, user-friendly assessment tool that delivers a clear overview of the sensitivity of reactions to key parameters is highly desirable. Herein, the development of such a method is described. The intuitive, standardized presentation of the results in a radar diagram enables the sensitivity of a protocol to be rapidly assessed.

Influence of barrier interlayers on the performance of Mo/Be multilayer mirrors for next-generation EUV lithography.

A comparative study was carried out of the structure and reflection performance of four types of multilayer mirror for extreme ultraviolet lithography at 11.2 nm; these were a pure Mo/Be structure and three Mo/Be-based structures with thin BC, C and Si interlayers. It was demonstrated that Mo/Be mirrors show maximum reflectance at normal incidence, while maximum structural perfection is shown by Mo/Be/Si mirrors.

Stable high-reflection Be/Mg multilayer mirrors for solar astronomy at 30.4 nm.

The He-II (λ=30.4  nm) emission line is one of the spectral channels chosen to study solar corona. This Letter reports on investigations of novel beryllium (Be)/magnesium multilayer coatings which, when incorporated beneath a protective bilayer of aluminium and Be, ensure particularly high-reflection coefficients of up to 56%, a spectral width of Δλ=1.

Soft X-ray Reflection Spectroscopy for Nano-Scaled Layered Structure Materials.

We introduce a novel approach that addresses the probing of interfacial structural phenomena in layered nano-structured films. The approach combines resonant soft x-ray reflection spectroscopy at grazing incidence near the "critical angle" with angular dependent reflection at energies around the respective absorption edges. Dynamic scattering is considered to determine the effective electron density and hence chemically resolved atomic profile across the structure based on simultaneous data analysis.

Diastereoselective Allylation of Aldehydes by Dual Photoredox and Chromium Catalysis.

Herein, we report the redox-neutral allylation of aldehydes with readily available electron-rich allyl (hetero-) arenes, β-alkyl styrenes and allyl-diarylamines. This process was enabled by the combination of photoredox and chromium catalysis, which allowed a range of homoallylic alcohols to be prepared with high levels of selectivity for the anti diastereomer. Mechanistic investigations support the formation of an allyl chromium intermediate from allylic C(sp)-H bonds and thus significantly extends the scope of the venerable Nozaki-Hiyama-Kishi reaction.

In Water and under Mild Conditions: α-Alkylation of Ketones with Alcohols by Phase-Transfer-Assisted Borrowing Hydrogen Catalysis.

Borrowing hydrogen is a powerful and green technique that allows readily available alcohols to be used as alkylating agents and produces water as the only by-product. Nevertheless, harsh conditions such as high temperatures and organic solvents are usually required. Herein, we present a strategy to perform the α-alkylation of ketones in aqueous media at mild temperatures by combining borrowing hydrogen with phase-transfer catalysis.

Total Synthesis of (+)-Pleuromutilin.

An 18-step synthesis of the antibiotic (+)-pleuromutilin is disclosed. The key steps of the synthesis include a highly stereoselective SmI-mediated cyclization to establish the eight-membered ring and a stereospecific transannular [1,5]-hydrogen atom transfer to set the C10 stereocenter. This strategy was also used to prepare (+)-12-epi-pleuromutilin.

Efficient high-order suppression system for a metrology beamline.

High-quality metrology with synchrotron radiation requires in particular a very high spectral purity of the incident beam. This is usually achieved by a set of transmission filters with suitable absorption edges to suppress high-order radiation of the monochromator. The at-wavelength metrology station at a BESSY-II bending-magnet collimated plane-grating monochromator (c-PGM) beamline has recently commissioned a high-order suppression system (HiOS) based on four reflections from mirrors which can be inserted into the beam path.

Gratings for synchrotron and FEL beamlines: a project for the manufacture of ultra-precise gratings at Helmholtz Zentrum Berlin.

Blazed gratings are of dedicated interest for the monochromatization of synchrotron radiation when a high photon flux is required, such as, for example, in resonant inelastic X-ray scattering experiments or when the use of laminar gratings is excluded due to too high flux densities and expected damage, for example at free-electron laser beamlines. Their availability became a bottleneck since the decommissioning of the grating manufacture facility at Carl Zeiss in Oberkochen. To resolve this situation a new technological laboratory was established at the Helmholtz Zentrum Berlin, including instrumentation from Carl Zeiss.

High-reflection Mo/Be/Si multilayers for EUV lithography.

The effect of Be layers on the reflection coefficients of Mo/Be/Si multilayer mirrors in the extreme ultraviolet (EUV) region is reported. Samples were studied using laboratory and synchrotron based reflectometry, and high-resolution transmission electron microscopy. The samples under study have reflection coefficients above 71% at 13.

Imidazole-stabilized, electron-deficient boron cations.

The borenium cations [(CHNAd)B(CF)][AlCl/AlCl] 2a, and [(CHNMe)B(CF)][B(CF)] 2b were prepared and are shown to feature a high Lewis acidity, the capability to activate hydrogen and to effect the 1,1-carborations of terminal and internal alkynes under mild conditions.

Impact of BC co-sputtering on structure and optical performance of Cr/Sc multilayer X-ray mirrors.

The influence of BC incorporation during magnetron sputter deposition of Cr/Sc multilayers intended for soft X-ray reflective optics is investigated. Chemical analysis suggests formation of metal: boride and carbide bonds which stabilize an amorphous layer structure, resulting in smoother interfaces and an increased reflectivity. A near-normal incidence reflectivity of 11.

Highly efficient blazed grating with multilayer coating for tender X-ray energies.

For photon energies of 1 - 5 keV, blazed gratings with multilayer coating are ideally suited for the suppression of stray and higher orders light in grating monochromators. We developed and characterized a blazed 2000 lines/mm grating coated with a 20 period Cr/C- multilayer. The multilayer d-spacing of 7.

At-wavelength metrology facility for soft X-ray reflection optics.

A new Optics Beamline coupled to a versatile UHV reflectometer is successfully operating at BESSY-II. It is used to carry out at-wavelength characterization and calibration of in-house produced gratings and novel nano-optical devices as well as mirrors and multilayer systems in the UV and XUV spectral region. This paper presents most recent commissioning data of the beamline and shows their correlation with initial beamline design calculations.

Potential Remedies for the High Synchrotron-Radiation-Induced Heat Load for Future Highest-Energy-Proton Circular Colliders.

We propose a new method for handling the high synchrotron radiation (SR) induced heat load of future circular hadron colliders (like FCC-hh). FCC-hh are dominated by the production of SR, which causes a significant heat load on the accelerator walls. Removal of such a heat load in the cold part of the machine, as done in the Large Hadron Collider, will require more than 100 MW of electrical power and a major cooling system.

The at-wavelength metrology facility for UV- and XUV-reflection and diffraction optics at BESSY-II.

A technology center for the production of high-precision reflection gratings has been established. Within this project a new optics beamline and a versatile reflectometer for at-wavelength characterization of UV- and XUV-reflection gratings and other (nano-) optical elements has been set up at BESSY-II. The Plane Grating Monochromator beamline operated in collimated light (c-PGM) is equipped with an SX700 monochromator, of which the blazed gratings (600 and 1200 lines mm(-1)) have been recently exchanged for new ones of improved performance produced in-house.