Search results for "thermal [correlation function]"

Kristallstruktur, thermische Ausdehnung und Farbwechsel von (Me3Ge)2Sb-Sb(GeMe3)2 und anderen Distibanen

1989

Abstract Single crystals of the distibanes (Me3M)4Sb2 (1: M = Si, 2: M = Ge) are obtained by the oxidation in air of (Me3M)3Sb. The crystal structure of 2 is reported. 2 forms linear chains of distibane molecules in trans conformation with Sb ··· Sb contacts of 386 pm at −110°C and 390 pm at 22°C. The thermal expansion of crystals of 2 and (Me3Sn)4Sb2 (3) has been determined. UV-VIS spectra of 1–3, Me4Sb2 (4), Et4Sb2 (5), and Ph4Sb2 (6) in different phases have been recorded. The spectra of 1–5 are consistent with the visible colour changes.

A novel oxovanadate structural type – Synthesis, single crystal structure and magnetic properties of a mixed-valence polyoxovanadate formed by {V17O4…

2007

Abstract A novel polyoxovanadate structural type, with an average nuclearity of V16, formed by a mixture of two different polyoxovananadates: {V15O36(Cl)} and{V17O40(Cl)} has been synthesized and characterized. The title compound, formulated as [Ni(phen)3]2{[V15O36(Cl)]0.5[V17O40(Cl)]0.5} · H2O (1) (phen = 1,10′-phenanthroline), presents two different polyoxovanadate architectures: {V15O36(Cl)} and {V17O40(Cl)}, with the last one representing a new framework type in polyoxovanadate chemistry. Here, we present the synthesis of this novel polyoxovanadate under hydrothermal conditions and its characterization by IR and XPS spectroscopies, elemental and thermogravimetric analysis, redox titrati…

K2AuPS4, TI2AuPS4, K2AuAsS4, and KAu5P2S8: Syntheses, structures, and properties of quaternary gold thiophosphate and thioarsenate compounds

1998

The novel compounds K2AuPS4 (1), Tl2AuPS4 (2), K2AuAsS4 (3), and KAu5P2S8 (4) have been synthesized by direct reaction of the elements with a molten alkaline polythiophosphate(arsenate) flux at 550°C. The crystal structures of these compounds have been determined by single-crystal X-ray diffraction techniques. 1, 2, and 3 crystallize in the monoclinic space group P21/m. The structures of 1, 2, and 3 consist of infinite, one-dimensional anionic chains running along the crystallographic b axis. The chains are separated by potassium or thallium ions. Neighbouring Au atoms are bridged by MS43− tetrahedra (M = P, As) in a trans orientation. Compound 4 crystallizes in the space group P21/c. The a…

Exploring the Role of Intramolecular Interactions in the Suppression of Quantum Tunneling of the Magnetization in a 3d-4f Single-Molecule Magnet.

2021

Hydroxide-bridged FeIII4LnIII2 clusters having the general formula [Fe4Ln2(μ3-OH)2(mdea)6(SCN)2(NO3)2(H2O)2]·4H2O·2MeCN {Ln = Y (1), Dy (2), mdea = N-methyldiethanolamine} were synthesized and magnetically characterized. The thermal relaxation of the magnetization for 2 and the diluted FeIII4DyIIIYIII complex 3 (with and without applied field) has been analyzed. The diluted sample shows a dominant QTM at low temperatures that can be removed with a 0.15 T dc field. Both 2 and 3 show moderately high Ueff barriers and exhibit hysteresis loops until 5 K.

From nitrides to carbides: topotactic synthesis of the η-carbides Fe3Mo3C and Co3Mo3C

2004

The molybdenum bimetallic interstitial carbides Fe(3)Mo(3)C and Co(3)Mo(3)C have been synthesized by temperature-programmed reaction (TPR) between the molybdenum bimetallic interstitial nitrides Fe(3)Mo(3)N and Co(3)Mo(3)N and a flowing mixture of CH(4) and H(2) diluted in Ar. These compounds have been characterized by X-ray diffraction, laser Raman spectroscopy, elemental analysis, energy dispersive analysis of X rays, thermal analysis (in air) and scanning electron microscopy (field emission). Their structures have been refined from X-ray powder diffraction data. These carbides crystallize in the cubic system, space group Fd3m[a= 11.11376(6) and 11.0697(3)[Angstrom] for Fe and Co compound…

Hydrothermal Synthesis, Crystal Structure, and Magnetism of Na 2 [Ir(OH) 6 ] and its Dehydration to Na 2 IrO 3

2021

Snapshots of the Formation of NaTi3O6(OH)·2H2O Nanowires: A Time-Resolved XRD/HRTEM Study

2013

Layered titanates are important intermediates during the formation of TiO2-related nanostructures in hot concentrated base solution. Microwave-assisted hydrothermal techniques allow a time-resolved ex-situ analysis of the reaction in one-minute intervals by rapid heating and quenching followed by separation and structure analysis of the intermediates. By a combination of powder X-ray diffraction, high resolution electron microscopy (HRTEM), and selected area electron diffraction (SAED) the individual stages of the reaction could be identified. Sodium titanate nanosheets are formed within several minutes by digesting the crystalline TiO2-P25 precursor in NaOH. These nanosheets with a low sod…

Acid-Promoted Rearrangement of the Metalated Thienyl Rings in Dirhodium(II) Complexes with Thienyl Phosphines as Ligands

2006

Several mono- and bis-cyclometalated compounds have been prepared and characterized from the thermal reaction of dirhodium(II) tetraacetate and tris(2-thienyl)phosphine, P(2-C4H3S)3 (1), in toluene/acetic acid mixtures. In refluxing acetic acid, the mono-cyclometalated compound Rh2(O2CCH3)3[(2-C4H2S)P(2-C4H3S)2] (CH3CO2H)2 (2A) isomerizes to Rh2(O2CCH3)3[(3-C4H2S)P(2-C4H3S)2](CH3CO2H)2 (2B), which results from the selective rearrangement of the metalated ring from a 2-thienyl to a 3-thienyl structure. In the same conditions, the bis-cyclometalated compounds of formula Rh2(O2CCH3)2[(2-C4H2S)P(2-C4H3S)2]2(CH3CO2H)2 and with head-to-tail (3AA) or head-to-head (4AA) configuration of the phosphi…

Kinetische Untersuchungen zu Diels‐Alder‐Reaktionen des Cyclooctins mit anschließender Aromatisierung

1984

Aus Cyclooctin (1) und den cyclischen Dienen 2a – g entstehen die Tricyclen 3a – g, die ganz unterschiedliche Stabilitat aufweisen. 3a, b, f und g zerfallen spontan. Unter Abspaltung von CO2, SO2, CO und N2 entstehen die aromatischen Verbindungen 4a – c. 3c eliminiert beim Erhitzen C2H4. 3e wird thermisch kaum mehr gespalten, aber ganz effizient bei der Photolyse, und 3d ist schlieslich gegenuber einer Aromatisierung stabil. Die thermische Ethylenabspaltung und die doppelte Photodecarbonylierung werden kinetisch untersucht. Kinetic Investigations of Diels-Alder-Reactions of Cyclooctyne with Consecutive Aromatization The tricyclic compounds 3a – g, generated from cyclooctyne (1) and the cycl…

Thermally highly stable amorphous zinc phosphate intermediates during the formation of zinc phosphate hydrate.

2015

The mechanisms by which amorphous intermediates transform into crystalline materials are still poorly understood. Here we attempt to illuminate the formation of an amorphous precursor by investigating the crystallization process of zinc phosphate hydrate. This work shows that amorphous zinc phosphate (AZP) nanoparticles precipitate from aqueous solutions prior to the crystalline hopeite phase at low concentrations and in the absence of additives at room temperature. AZP nanoparticles are thermally stable against crystallization even at 400 °C (resulting in a high temperature AZP), but they crystallize rapidly in the presence of water if the reaction is not interrupted. X-ray powder diffract…