Abstract The combination of two analytical methods including time‐resolved in situ X‐ray diffraction (XRD) and Raman spectroscopy provides a new opportunity for detailed analysis the key mechanisms milling reactions. To prove general applicability our setup, we investigated mechanochemical synthesis four archetypical model compounds, ranging from 3D frameworks through layered structures to organic molecular compounds. reaction mechanism each compound could be elucidated. results clearly show...

We present a first direct measurement of the temperature during milling combined with<italic>in situ</italic>Raman spectroscopy monitoring.

Abstract The combination of two analytical methods including time‐resolved in situ X‐ray diffraction (XRD) and Raman spectroscopy provides a new opportunity for detailed analysis the key mechanisms milling reactions. To prove general applicability our setup, we investigated mechanochemical synthesis four archetypical model compounds, ranging from 3D frameworks through layered structures to organic molecular compounds. reaction mechanism each compound could be elucidated. results clearly show...

The structure and the formation pathway of a new theobromine : oxalic acid (2 1) cocrystal are presented.

Two metal organic structures composed of the ligands benzene-1,4-dicarboxylate and pyridine-2,5-dicarboxylate bismuth cations are presented: (H₂Im)[Bi(1,4-bdc)₂] (<bold>1</bold>) [Bi(pydc)(NO₃)₂(H₂O)₂]·H₂O (<bold>2</bold>) (bdc = benzenedicarboxylate, H₂Im imidazole cation, pydc pyridinedicarboxylate).

New and known cadmium phenylphosphonates were prepared mechanochemically their synthesis mechanism was determined<italic>in situ</italic>.

Abstract The in situ investigations of the mechanochemical synthesis four hybrid organic–inorganic lead(II) iodides with formula (C(NH 2 ) 3 n PbI 2+ ( n= 1 , and 4 are presented. Synchrotron X‐ray diffraction data show that guanidinium easily convert into each other. Although end product is dictated by initial stoichiometry, complex pathways were found different behaviors compounds terms nucleation, growth, intermediate formation. This appears to be linked respective structural features...

We describe a fast and effective synthesis for molecular metal phosphonates. Isomorphic compounds [M(ii)(HO3PPh)2(H2O3PPh)2(H2O)2] (M = Mn (1), Co (2), Ni (3); Ph C6H5) were obtained by grinding. The complexes are mononuclear containing neutral monodeprotonated phenylphosphonic acid water as ligands. crystal structures determined using powder X-ray diffraction (PXRD) data validated extended absorption fine structure (EXAFS) data. Combined synchrotron XRD measurements Raman spectroscopy...

Time-resolved mechanochemical cocrystallisation studies have so-far focused solely on neat and liquid-assisted grinding. Here, we report the investigation of polymer-assisted grinding reactions using in situ X-ray powder diffraction, revealing that reaction rate is almost double compared to independent molecular weight amount polymer additive used.

<italic>In situ</italic> investigation and elucidation of the formation a POM@MOF host guest system obtained by mechanosynthesis.

The controlled synthesis of superparamagnetic iron oxide nanoparticles is crucial for a variety biomedical applications. Among different routes, thermal precursor decomposition methods are the most versatile, yielding monodisperse on multigram scale. Recent in situ kinetic studies nucleation and growth processes during routes revealed nonclassical paths involving amorphous phases aggregative steps. With knowledge this mechanism, we systematically examined range heat-up to understand conclude...

Crystalline arrays of the gastric H,K-ATPase were obtained in membrane preparations from hog and rabbit mucosa.The lattice was formed rapidly a medium containing K', vanadate, Mg"', dimethyl sulfoxide at pH 6.0-6.9 imidazole buffer 4 to 22 "C.The crystal exhibited P2 symmetry, unit cell dimension (a = 5.6, b 11, c 10 nm) could accommodate 2 polypeptides mass 116-129 kDa.In addition, isolated preparation contained previously undescribed long cylindrical structures 16 nm thick.These consisted...

Zn and Zn-TiO2 coatings were galvanostatically electrodeposited on steel substrates from chloride- sulfate-plating baths. The influence of the electrolyte type dispersion behavior TiO2 nano-particles as well amount incorporation was studied. electrokinetic titania in diluted electrolytes is strongly influenced by specific adsorption SO42− anions. Chemical depth profile analysis using glow discharge optical emission spectroscopy confirmed particles throughout layers (up to 0.53 wt% 0.78...

Mechanochemistry offers a new route to polyoxometalates (POMs) under mild conditions. The molybdenum isoPOM heptamolybdate and the heteroPOMs of Strandberg- Keggin-type could be achieved from grinding together oxide, potassium or ammonium carbonate phosphate. reactions were controlled by stoichiometric ratio starting materials liquid used, with reaction times between 30 min 3 h. In situ investigations syntheses reveal formation intermediates during reactions. Their identification helps...

The crystal structures and syntheses of four different copper(ii) phenylphosphonates, the monophenylphosphonates α-, β-, γ-Cu(O3PC6H5)·H2O (α-CuPhPmH (1) β-CuPhPmH (2) γ-CuPhPmH (3)), diphosphonate Cu(HO3PC6H5)2·H2O (CuPhP2mH (4)), are presented. compounds were synthesized from solution at room temperature, elevated under hydrothermal conditions, mechanochemical conditions. α-CuPhPmH CuPhP2mH (4) solved powder X-ray diffraction data. structure was by single analysis. validated extended...

We present a series of remarkable structural transformations for family layered metal–organic frameworks (MOFs) in three-step solid-state reaction cycle. The cycle represents new dynamic behavior 2D coordination polymers and involves the sequence reactions: {[Mn2(ina)4(H2O)2]·2EtOH}n (JUK-1) → {(NH4)2[Mn(ina)2(NCS)2]}n·xH2O (JUK-2) {[Mn2(ina)2(Hina)2(NCS)2]}n (JUK-3) JUK-1 (Hina = isonicotinic acid), each accompanied by rearrangement intralayer bonds induced different external stimulus. In...

Abstract Divalent metal phosphonates are promising hybrid materials with a broad field of application. The rich coordination chemistry the phosphonate linkers enables formation structures different dimensionalities ranging from isolated complexes and layered to porous frameworks incorporating various functionalities through choice building blocks. In brief, offer an interesting opportunity for design multifunctional materials. Here, we provide short review on class divalent discussing their...

Structure-properties relationship of new Cd-benzylphosphonates differing in their fluorine content.

The influence of sulfur compounds on the vaporization sodium from soda‐lime‐silica glass was investigated using newly developed stirrable transpiration apparatus (STA). With increasing concentration in either melt or atmosphere above it, sodium‐vapor density found to increase until attaining value over pure sodium‐sulfate liquid. At that point, became independent concentration, presumably due separation liquid glass. Since behavior containing similar molten Na 2 SO 4 , thermodynamically...

Abstract The mechanism for the mechanochemical synthesis of (C(NH 2 ) 3 PbI 5 and 4 6 their conversion into each other is presented. We investigated at different frequencies energies using in situ powder X‐ray diffraction. By splitting reaction single parts we could prove that formation simply dependent on energy mixing speed. nucleation instead slightly negative but speed, while its growth mostly independent any influence. were able to influence pathways by seeding mixture with a small...