Synthesis Of Cs Research Articles

Chemical and Phase Transformations during the Synthesis of Cs[MgR0.5P1.5O6] (R = B, Al, Fe) Complex Oxides from Metal Nitrates

Chemical and Phase Transformations during the Synthesis of Cs[MgR0.5P1.5O6] (R = B, Al, Fe) Complex Oxides from Metal Nitrates

Synthesis and Crystal Structure of Cs2U2(P2Se9)(Se2)2

Black single crystals of Cs2U2(P2Se9)(Se2)2 were synthesized at 1023 K by a solid‐state reaction. Its structure was determined by single‐crystal X‐ray diffraction methods. The compound is isostructural with Rb2U2(P2Se9)(Se2)2 and Cs2Th2(P2Se9)(Se2)2 compounds, and crystallizes in the orthorhombic space group Pbca. Cs2U2(P2Se9)(Se2)2 displays a three‐dimensional structure comprising USe9 polyhedra connected via the Se22– and P2Se9 species with channels filled by Cs atoms. From electronic structure calculations the compound is found to be a metal with a ferromagnetic arrangement of the magnetic moments.

Chemical and Phase Transformations during the Synthesis of Cs[MgR0.5P1.5O6] (R = B, Al, Fe) Complex Oxides from Metal Chlorides

Cesium-containing complex oxides Cs[MgR0.5P1.5O6] (R = B, Al, Fe) are prepared from solutions containing H3BO3, metal chlorides, and H3PO4/NH4H2PO4. The chemical and phase transformations that occur during the synthesis are elucidated by differential thermal analysis (DTA) and X-ray powder diffraction (XRD). Optimal synthesis parameters are determined. The oxides where R = B or Fe are formed at 800°C, those where R = Al are formed at 1100°C. All compounds crystallize in the pollucite-type structure (cubic system, space group I4132).

Synthesis and characterization of a novel peptide-grafted Cs and evaluation of its nanoparticles for the oral delivery of insulin, in vitro, and in vivo study.

BackgroundDespite years of experience and rigorous research, injectable insulin is the sole trusted treatment method to control the blood glucose level in diabetes type 1 patients, but injection of insulin is painful and poses a lot of stress to the patients, especially children, therefore, development of a non-injectable formulation of insulin is a major breakthrough in the history of medicine and pharmaceutical sciences.MethodsIn this study, a novel peptide grafted derivative of chitosan (CPP-g- chitosan) is synthesized and its potential for oral delivery of proteins and peptides is evaluated. Drug-loaded nanoparticles were developed from this derivative using ionic gelation method with application of sodium tripolyphosphate (TPP) as a cross-linking agent. Human insulin was used as the model protein drug and release kinetic was studied at gastrointestinal pH. Finally the developed nanoparticles were filled into very tiny enteric protective capsules and its effects on blood glucose level are evaluated in laboratory animals.ResultsPresence of the positively charged cell-penetrating peptide moiety in the structure of chitosan polymer had slight inhibitory effects on the release of insulin from the nanoparticles in simulated gastric fluid (pH 1.2) comparing to native chitosan. The nanoparticles were positively charged in gastrointestinal pH with size ranging from 180 nm to 326 nm. The polypeptide grafted to chitosan is a novel analog of Penetratin, presenting both the hydrophilic and hydrophobic characteristics altering the release behavior of the nanoparticles and significantly increase the absorption of insulin into the rat epithelium comparing to nanoparticles from simple chitosan. In-vivo results in diabetic rat proved that this nanoparticulate system can significantly lower the blood glucose levels in diabetic rats and remain effective for a duration of 9–11 hours.ConclusionThe results indicate that nanoparticles developed from this new peptide conjugated derivative of chitosan are very promising for oral delivery of proteins and peptides.

Controllable synthesis of small size CsxWO3nanorods as transparent heat insulation film additives

Small size CsxWO3nanorods synthesized using pure ethanol as the solvent exhibited the best visible transparency and NIR shielding performance.

High-pressure-assisted X-ray-induced damage as a new route for chemical and structural synthesis.

X-ray induced damage has been known for decades and has largely been viewed as a tremendous nuisance. We, on the other hand, harness the highly ionizing and penetrating properties of hard X-rays to initiate novel decomposition and synthetic chemistry. Here, we show that powdered cesium oxalate monohydrate pressurized to ≤0.5 GPa and irradiated with X-rays of energies near the cesium K-edge undergoes molecular and structural transformations with one of the final products exhibiting a new type of bcc crystal structure that has previously not been observed. Additionally, based on cascades of ultrafast electronic relaxation steps triggered by the absorption of one X-ray photon, we propose a model explaining the X-ray induced damage of multitype bounded matter. As X-rays are ubiquitous, these results show promise in the preparation of novel compounds and novel structures that are inaccessible via conventional methods. They may offer insight into the formation of complex organic compounds in outer space.

Cu and Zn Substituted Silicon Clathrates with the Cubic Type‐II Structure: Synthesis and Characterization of Cs8Na16Cu3.8Si132.2 and Cs8Na16Zn6.9Si129.1

Studies in the systems Cs–Na–Cu–Si and Cs–Na–Zn–Si yielded the novel clathrates Cs8Na16(Cu,Si)136 and Cs8Na16(Zn,Si)136, both with the cubic type‐II structure [space group Fd3m (no. 227), Pearson symbol cF160]. The structures of the title compounds were established from single‐crystal X‐ray diffraction methods, confirming the complete ordering of the Cs and Na guest atoms. The framework‐building Si atoms are found to be randomly substituted by Cu atoms on framework site 96g, exclusively. In the structure of Cs8Na16(Zn,Si)136, the refinements indicate that the Zn and Si atoms co‐occupy two of the three framework sites with notable preference for site 96g over site 32e. The corresponding refined compositions and unit cell parameters are as follows: Cs8Na16Cu3.8Si132.2(1) [a = 14.7583(15) Å]; Cs8Na16Zn6.9Si129.1(1) [a = 14.7682(5) Å], respectively. The type‐II clathrates can be obtained only from experiments employing both Na and Cs, whereas work in the ternary Cs‐Cu‐Si, Cs‐Zn‐Si, Na‐Cu‐Si, and Na‐Zn‐Si systems failed to yield any clathrate phases. At the same conditions, exploratory studies in the K‐Zn‐Si and Rb‐Zn‐Si systems provided evidence that type‐I clathrates are favored.

Taming the High Reactivity of Gold(III) Fluoride: Fluorido Gold(III) Complexes with N‐Based Ligands

The synthesis of [NMe4 ][AuF4 ] and [NEt4 ][AuF4 ], as well as an improved one-pot synthesis of Cs[AuF4 ], is reported. The new [AuF4 ]- salts were structurally characterized by single crystal X-ray diffraction, NMR spectroscopy, vibrational spectroscopy, and mass spectrometry. These salts are the first gold(III) fluoride salts that can be isolated in pure form and are convenient to be used in usual organic solvents for subsequent synthesis. The formation of molecular AuF3 complexes in solution is further reported, characterized as [F3 Au(NCCH3 )] at low temperature, as [F3 Au(py)] and a binuclear derivative which are stable at room temperature. The stability of these species in common organic solvents was investigated and they showed a satisfying stability.

A [Mo2O2S2]-based ring system incorporating tartrate as the bridging ligand: synthesis, structure and catalytic activity of Cs4[Mo2O2(μ-S)2]2(μ4-tart)2 (tart=[C4H2O6]4−)

Abstract Treatment of [Mo2S2O2(H2O)6]2+ with racemic tartaric acid (tartH4) in the presence of sodium hydroxide and cesium chloride in aqueous solution led to the isolation of a new tetra-molybdenum ring cluster Cs4[Mo2O2(μ-S)2]2(μ4-tart)2. The cyclic cluster polyanion consists of two dinuclear [Mo2O2(μ-S)2]2+ moieties and two bridging tart4− ligands. The cyclic polyoxothiomolybdate cluster, supported on the mesoporous silica SBA-15, was tested for heterogenerous catalysis in thiophene hydrodesulfurization.

Ammonothermal Synthesis and Characterization of Cs2[Zn(NH2)4

Cs2[Zn(NH2)4] was synthesized under ammonothermal conditions (sc‐NH3, 523 K, 155 MPa) from CsNH2 and Zn. Growth of cm‐sized crystals succeeded upon application of a temperature gradient. The crystal structure is based on the motif of a hexagonal closed packing of [Zn(NH2)4]2– ions with occurrence of no significant hydrogen bridges according to distances and vibrational spectroscopy. Cs+ ions are located within octahedral and tetrahedral holes of the packing.

Cover Picture: Ammonothermal Synthesis and Characterization of Cs2[Zn(NH2)4] (Z. Anorg. Allg. Chem. 21/2016)

Cover Picture: Ammonothermal Synthesis and Characterization of Cs₂[Zn(NH₂)₄] (Z. Anorg. Allg. Chem. 21/2016)

Progress in Polyarsolyl Chemistry.

The synthesis of heteroatom analogues of the cyclopentadienyl anion Cp− is a fascinating and challenging field of research. The replacement of methine moieties by phosphorus is well investigated for the synthesis of mono‐, tri‐ and pentaphospholyl ligands. On the other hand, arsenic derivatives are rare and 1,2,4‐triarsolyl and tetraarsolyl salts are unknown. Herein, we report on the synthesis of Cs[E3C2(trip)2] (1 a: E=P; 1 b: E=As; trip=2,4,6‐triisopropylphenyl) and Cs[E4C(trip)] (2 a: E=P; 2 b: E=As). Compound 1 b represents the first 1,2,4‐triarsolyl and 2 b the first tetraarsolyl anion. All salts are obtained in one‐pot syntheses using E(SiMe3)3, 2,4,6‐triisopropylbenzoyl chloride and CsF. The products 1 a⋅2 C4H8O2, 2 a⋅Et2O and 2 b⋅3 C4H8O2 were characterized by X‐ray structural analysis, which revealed planar heterocycles. Nucleus‐independent chemical shifts (NICS) confirmed the aromaticity of these anions. Notably, compound 2 a⋅Et2O is only the second tetraphospholyl ligand which is structurally characterized.

Synthesis of the Layered Quaternary Uranium-Containing Oxide Cs2Mn3U6O22 and Characterization of its Magnetic Properties.

A layered quaternary uranium-containing oxide, Cs2Mn3U6O22, was crystallized from a cesium chloride flux. The crystal structure was determined to consist of α-U3O8 topological layers that are separated by alternating cesium and manganese layers. This ordered arrangement creates a separation between manganese layers of 13 Å, leading to complex low-dimensional magnetic properties. The compound crystallizes in a new structure type in the monoclinic space group, C2/m, with a = 6.8730(10) Å, b = 11.7717(17) Å, c = 13.374(2) Å, and β = 99.673(5)°. The magnetic properties were measured and analyzed by first-principles density functional theory calculations.

ChemInform Abstract: Synthesis, Structural Characterization, and Physical Properties of Cs2Ga2S5, and Redetermination of the Crystal Structure of Cs2S6.

AbstractCs2Ga2S5 is prepared by slow thermal decomposition of CsN3 in presence of stoichiometric amounts of GaS and S in dynamic vacuum followed by annealing (quartz tube, 803 K, several d).

Synthesis, characterization and thermochemistry of Cs-, Rb- and Sr-substituted barium aluminium titanate hollandites

Titanate hollandites are of considerable interest for immobilization of radioactive Cs, its daughter product Ba and related radionuclides Rb and Sr. In this study, we synthesized three hollandites, Ba1.18Cs0.21Al2.44Ti5.53O16, Ba1.17Rb0.19Al2.46Ti5.53O16 and Ba1.14Sr0.10Al2.38Ti5.59O16, using sol–gel methods. Rietveld analysis of synchrotron XRD data shows that they adopt the tetragonal structure (space group I4/m), and their cell parameters increase with increasing cation size (Sr2+→Rb+→Cs+). Standard enthalpies of formation of these hollandites were determined from drop solution calorimetric measurements with lead borate as the solvent at 973K. Their formation enthalpies are similar, consistent with the occurrence of extensive cation substitutions in hollandites. Further energetic analysis with respect to BaTiO3 and SrTiO3 perovskites and other oxides reveals decreased thermodynamic stability from Cs- to Rb- to Sr-hollandite. This trend is consistent with the phase assemblage observed in Synroc, where Cs+, Rb+ and Ba2+ enter into hollandite, whereas Sr2+ occurs in perovskite.

Toward p-type conduction in Cs-doped ZnO: an eco-friendly synthesis method

An alcohol-free, eco-friendly technique was adapted for the synthesis of undoped ZnO and Cs-(cesium) doped ZnO nanoparticles (NPs). The effect of annealing and dopant concentration on its structural and optical properties was investigated. X-ray diffraction results confirmed the formation of polycrystalline hexagonal wurtzite structure and enhanced crystallinity was observed for 1 mol%: Cs-doped ZnO NPs. Scanning electron microscopy results revealed triangular-shaped NPs and increase in the crystallite size is noticed with increase in dopant concentration. UV–visible results showed shift in the band edge toward higher wave length side with increasing Cs concentration. Reduction in bandgap was observed for Cs-doped ZnO NPs, due to quantum confinement effect. Transmittance value increased to 86 % with the inclusion of Cs in ZnO lattice. Room temperature photoluminescence analysis of Cs-doped ZnO NPs reveals bandedge emission along with 450 nm emission due to Zn vacancy and Zn interstitial defects. Electrical measurements confirmed the realization of p-type conductivity in Cs-doped ZnO NPs with a carrier concentration of 1.3 × 1018/cm3.

Synthesis and reactivity of new functionalized perfluoroalkylfluorophosphates.

A new efficient synthesis of functionalized perfluoroalkyl fluorophosphates by oxidative addition of Me2NCH2F to the electron-deficient phosphanes (C2F5)(n)PF(3-n) (n=0-3) is reported. The initially formed zwitterionic, hexacoordinated phosphates [(C2F5)(n)F(5-n)P(CH2NMe2-CH2NMe2)] are converted into the corresponding phosphonium salts [(Me3PCH2NMe2](+)[(C2F5)(n)F(5-n)P(CH2NMe2)](-) by treatment with PMe3. In addition [(C2F5)3F2P(CH2NMe2-CH2NMe2)] can undergo a 1,3-methyl shift from the internal to the terminal nitrogen--a structural characterization was achieved from the CF3 analogue. Reaction of [(C2F5)3F2P(CH2NMe-CH2NMe3)] and PMe3 gave rise to the formation of the zwitterionic phosphonium phosphate [(C2F5)3F2P(CH2NMe-CH2PMe3)], which was fully characterized by X-ray diffraction analysis. Moreover, an efficient one-pot synthesis of Cs(+)[(C2F5)3F2P(CH2NMe2)](-) was pursued. This salt turned out to be a useful nucleophile in several alkylation reactions.

Synthesis of face-centred cubic Cs3C60in THF

A solution chemistry synthetic route yields Cs(3)C(60) with a face-centred cubic structure. The described method uses well-established Schlenk techniques and THF as a solvent. The controlled addition of an organo-metallic salt reducing agent prevents the formation of C(60)(4-) salts. The final product can be precipitated from the solution using hexane as an anti-solvent.

ChemInform Abstract: Unprecedented Electron‐Poor Octahedral Ta6 Clusters in a Solid‐State Compound: Synthesis, Characterizations and Theoretical Investigations of Cs2BaTa6Br15O3.

AbstractCs2BaTa6Br15O3 and Cs2LaTa6Br15O3 are obtained from stoichiometric mixtures of Ta, Ta2O5, TaBr5, CsCl, and BaBr2 or La2O3 (sealed silica container, 650—690 °C, 3 d).

ChemInform Abstract: High Temperature Redox Reactions with Uranium: Synthesis and Characterization of Cs(UO2)Cl(SeO3), Rb2(UO2)3O2 (SeO3)2, and RbNa5U2(SO4)7.

AbstractCs(UO2)Cl(SeO3) (I) and Rb2(UO2)3O2 (SeO3)3 (II) are prepared by melting stoichiometric amounts of UO2 and SeO2 together with excess CsCl or RbCl both as cation source and fluxing agent (evacuated silica ampoules, 850 °C, 5 d).