The quality of diffraction data obtained using silver and molybdenum microsources has been compared for six model compounds with a wide range absorption factors. experiments were performed on two 30 W air-cooled Incoatec IµS microfocus sources multilayer optics mounted Bruker D8 goniometer SMART APEX II CCD detector. All analysed, processed refined standard software. results show that Ag

Molecular encapsulation processes under the control of an external trigger play a major role in biological signal transduction and enzyme catalysis. Here, we present artificial mimic controllable host system that forms via self-assembly from simple bis-monodentate ligand Pd(II) cations. The resulting interpenetrated double cage features three consecutive pockets which initially contain one tetrafluoroborate anion, each. Activation this with two halide anions triggers conformational change...

Irradiation of rhodium(II) azido complex [Rh(N3){N(CHCHPtBu2)2}] allowed for the spectroscopic characterization first reported rhodium with a terminal nitrido ligand. DFT computations reveal that unpaired electron rhodium(IV) nitride [Rh(N){N(CHCHPtBu2)2}] is located in an antibonding Rh-N π* bond involving moiety, thus resulting predominant N-radical character, turn providing rationale its transient nature and observed coupling to dinitrogen.

The synthesis and characterization of a new kind cis- trans-cyclometalated square-planar platinum(II) complexes is reported. Uncharged organometallic compounds carrying one or two the C∧N-donor ligand LCN were prepared. Due to heterobidentate coordination achiral chelate ligand, formed [PtLCNCl(SEt2)], trans-[PtLCN2] are chiral with metal serving as stereo center. enantiomers complex could be separated their absolute configuration was determined by anomalous X-ray diffraction, in accordance...

Low-energy contamination caused by focusing multilayer optics has been known for a long time. So far, the only method to avoid this problem is attenuation interposition of low-density material foil into beam. However, lowers intensity, which might be crucial, especially charge density data collection, and course not possible already measured data. In article, an empirical correction proposed as alternative or addition. The low-energy mainly affects reflections with indices 3 h k l . program...

Previously, we introduced a series of anion-binding interpenetrated double-cages based on phenothiazine and its mono- di-S-oxygenated derivatives. Here, complete the structural comparison three related assemblies by an X-ray single crystal analysis sulfone derivative. We further show that palladium cages coexist in solution upon post-assembly mixing due to very slow ligand exchange whereas treatment binary mixtures corresponding ligands with Pd(II) leads formation mixed comprising...

Coordination polymers exhibiting mechanical flexibility including elastic or plastic bending are rare. Here, we report an example of a mechanically flexible one-dimensional coordination polymer that shows bending. Quantitative insights on the inter and intra-chain bonding as well structural from combination techniques variable temperature single crystal X-ray diffraction (XRD), high-pressure crystallography (ambient─15 GPa), synchrotron micro-XRD mapping bent crystal, high-resolution charge...

Hybrid photon-counting detectors are widely established at third-generation synchrotron facilities and the specifications of Pilatus3 X CdTe were quickly recognized as highly promising in charge-density investigations. This is mainly attributable to detection efficiency high-energy X-ray regime, combination with a dynamic range noise level that should overcome perpetual problem detecting strong weak data simultaneously. These benefits, however, come expense persistent for high diffracted...

A cross-validation method is supplied to judge between various strategies in multipole refinement procedures. Its application enables straightforward detection of whether the additional parameters leads an improvement model or overfitting given data. For all tested data sets it was possible prove that atoms comparable chemical environments should be constrained identical. In automated approach, this additionally delivers parameter distributions k different refinements. These can used for...

A silicon atom in the zero oxidation state stabilized by two carbene ligands is known as siladicarbene (silylone). There are pairs of electrons on silylone. This was recently confirmed both experimental and theoretical charge density investigations. The silylone stable up to 195 °C an inert atmosphere. However, a substoichiometric amount (33 mol%) potassium metal triggers activation unsaturated C:Si:C backbone, leading selective reaction with tertiary C-H bond atom-economical approach form...

Serial femtosecond crystallography for small-unit-cell systems has so far seen very limited application despite obvious scientific possibilities. This is because reliable data reduction not been available these challenging systems. In particular, important intensity corrections such as the partiality correction critically rely on accurate determination of crystal orientation, which complicated by low number diffraction spots crystals. A pipeline capable fully automated handling all steps...

The quality of various approximation methods for modelling anisotropic displacement parameters (ADPs) hydrogen atoms was investigated in a comparative study. A multipole refinement performed against high-resolution single crystal X-ray data 9-diphenylthiophosphoranylanthracene (SPAnH) and 9,10-bis-diphenylthiophosphoranylanthracene·toluene (SPAnPS). Hydrogen-atom structural properties derived from our collected neutron sets were compared with those obtained the SHADE -server, software...

Understanding magnetic anisotropy and specifically how to tailor it is crucial in the search for high-temperature single-ion magnets. Herein, we investigate a six-coordinated cobalt(II) compound that has complex geometry distinct triaxial from perspective of electronic structure, using spectra, ab initio calculations, an experimental charge density, which latter two provides insight into d-orbital splitting. The analysis showed splitting satisfactorily predicted exhibited by compound....

The first carbonyl free mixed valence cobalt(I)/cobalt(II) compound [2{L2Co(I)(η(6)-C7H8)}](2+) [Co(II)2Cl6](2-) (1) [L = PhC(N(t)Bu)2SiCl] was obtained by the reaction of four equivalents anhydrous CoCl2 with five N-heterocyclic chlorosilylene L. In contrast, L CoBr2 yielded [L2CoBr2] (2). Compound 1 formed cleavage Co-Cl bonds, reduction Co(II) to Co(I) and coordination a toluene molecule. (L) functions as reducing agent well neutral σ-donor ligand. molecule coordinates atom in an η(6)-fashion.

Abstract Reported here is an entirely new application of experimental electron density (EED) in the study magnetic anisotropy single‐molecule magnets (SMMs). Among those SMMs based on one single transition metal, tetrahedral Co II ‐complexes are prominent, and their large zero‐field splitting arises exclusively from coupling between d xy orbitals. Using very low temperature single‐crystal synchrotron X‐ray diffraction data, accurate (ED) was obtained for a prototypical SMM, d‐orbital...

Melamine is a precursor and building block for graphitic carbon nitride (g-CN) materials, group of layered materials showing great promise catalytic applications. The synthetic pathway to g-CN includes polycondensation reaction melamine by evaporation ammonia. molecules in the crystal organize into wave-like planes with an interlayer distance 3.3 Å similar that g-CN. Here we present extensive investigation experimental electron density obtained from modelling synchrotron radiation X-ray...

SrMn2P2 and CaMn2P2 are insulators that adopt the trigonal CaAl2Si2-type structure containing corrugated Mn honeycomb layers. Magnetic susceptibility χ heat capacity versus temperature T data reveal a weak first-order antiferromagnetic (AFM) transition at Néel [Formula: see text] K for strong AFM Both compounds exhibit isotropic nearly T-independent text], suggesting magnetic structures in which nearest-neighbor moments aligned to each other. The 31P NMR measurements confirm but show...

Five different electron density datasets obtained from conventional and synchrotron single crystal X-ray diffraction experiments are compared. The general aim of the study is to investigate quality data for analysis current state-of-the-art sources, see how perform in comparison with high-quality data. A molecular melamine was selected as test compound due its ability form excellent crystals, light atom content, an advantageous suitability factor 3.6 modeling. These features make optimal...

Single crystal synchrotron X-ray diffraction data are used to obtain an experimental electron density of a magnetic coordination polymer and thereby probe chemical interactions responsible for pathways.

Abstract Reported here is an entirely new application of experimental electron density (EED) in the study magnetic anisotropy single‐molecule magnets (SMMs). Among those SMMs based on one single transition metal, tetrahedral Co II ‐complexes are prominent, and their large zero‐field splitting arises exclusively from coupling between d xy orbitals. Using very low temperature single‐crystal synchrotron X‐ray diffraction data, accurate (ED) was obtained for a prototypical SMM, d‐orbital...

In this work, the magnetic anisotropy in two iso-structural distorted tetrahedral Co(II) complexes, Co X 2 tmtu [ = Cl( 1 ) and Br( ), tetramethylthiourea] is investigated, using a combination of polarized neutron diffraction (PND), very low-temperature high-resolution synchrotron X-ray CASSCF/NEVPT2 ab initio calculations. Here, it was found consistently among all methods that compounds have an easy axis magnetization pointing nearly along bisector compression angle, with minute deviations...

X-ray scattering data measured on femtosecond timescales at the SACLA Free Electron Laser (XFEL) facility a suspension of HfO2 nanoparticles in liquid jet were used for pair distribution function (PDF) analysis. Despite non-optimal experimental setup resulting modest Qmax ~8 Å-1 , promising PDF was obtained. The main features reproduced when comparing XFEL to obtained from PETRA III synchrotron light source. Refining structural parameters such as unit cell dimension and particle size...

xrdPlanner is a software package designed to aid in the planning and preparation of powder X-ray diffraction total scattering beam times at synchrotron facilities. Many modern beamlines provide flexible experimental setup may have several different detectors available. In combination with range available energies, it often makes difficult for user explore parameter space relevant given experiment prior scheduled time. was developed fast straightforward tool that allows users visualize...