Bismuth-rich bimetallic clusters (CuBi8)3+ and [MBi10]4+ (M = Pd, Pt) from ionothermal synthesis

2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Maximilian Knies ◽  
Michael Ruck
Keyword(s):  
Ionic Liquid ◽  
Bimetallic Clusters ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ionothermal Synthesis ◽  
Acidic Ionic Liquid ◽  
Metal Atoms ◽  
Cluster Cation ◽  
Complex Salts ◽  
Lewis Acidic Ionic Liquid

Abstract The reaction of Bi, BiBr3, and CuBr in the Lewis-acidic ionic liquid [BMIm]Br·4AlBr3 (BMIm = 1-n-butyl-3-limidazolium) at 180 °C yielded air-sensitive, shiny black crystals of (CuBi8)[AlBr4]2[Al2Br7]. Crystals of [MBi10][AlCl4]4 (M = Pd, Pt) were obtained by reacting Bi, BiCl3, and MCl2 under similar conditions. The structures have been determined by X-ray diffraction on single-crystals and were found to be very similar to that of the known analogues with other halogens, although not isostructural. In crystals of the complex salts, polyhedral bimetallic clusters (CuBi8)3+ or [MBi10]4+ are embedded in matrices of halogenidoaluminate anions. The heteroatomic nido-cluster (CuBi8)3+ consists of a (Bi8)2+ square antiprism η4-coordinating a copper(I) cation. In the cluster cation [MBi10]4+, the metal atoms M center a pentagonal antiprism of bismuth atoms.

Synthesis, Characterization, and Crystal Structure of Several Novel Acidic Ionic Liquids: 1-ethyl-2-alkyl-benzimidazolium Tetra-Fluoroborate

2013 ◽  
Vol 457-458 ◽  
pp. 139-143 ◽  
Author(s):  
Ming Tian Wang ◽  
Chang Ping Pan ◽  
Wei Peng Gai ◽  
Xiao Xia Lv ◽  
Min Gang Zhai ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Ionic Liquid ◽  
Acetic Acid ◽  
Catalytic Activity ◽  
Lamellar Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Acidic Ionic Liquid ◽  
Acidic Ionic Liquids ◽  
Good Catalytic Activity

A series of novel acidic ionic liquid: 1-ethyl-2-alkyl-benzimidazolium tetra-fluoroborate (alkyl= Et, Pr-n, Bu-n) were prepared by simple acid-based neutralization of 1-ethyl-2-alkyl-benzimidazole and tetrafluoroboric acid. The compounds were characterized by FTIR spectra, elemental analysis,1HNMR spectra and thermogravimetric analysis. These novel tetra-fluoroborate salts show good catalytic activity to esterification of benzyl alcohol and acetic acid. Furthermore, a crystal of ([H-ebBiBF4) was prepared with the crystal structure and determined by X-ray diffraction analysis. The molecular is of lamellar structure as mainly π electron ring is stacked interleaving between two layers. The results of cation and anion arranged orderly in pair indicate that the coulombic attraction is more dominant. Simultaneously, the weak local hydrogen bonds C-H···F exist in the molecules.

Salts of octabismuth(2+) polycations crystallized from Lewis-acidic ionic liquids

2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Maximilian Knies ◽  
Michael Ruck
Keyword(s):  
Room Temperature ◽  
Structure Type ◽  
Chloride Ions ◽  
X Ray Diffraction ◽  
Slow Cooling ◽  
X Ray ◽  
Acidic Ionic Liquid ◽  
Acidic Ionic Liquids ◽  
High Temperature Form ◽  
Lewis Acidic Ionic Liquid

Abstract The reaction of Bi and BiCl3 with RbCl or CsCl in the Lewis-acidic ionic liquid (IL) [BMIm]Cl·4AlCl3 at T = 200 °C yielded air-sensitive, shiny black crystals. X-ray diffraction on single crystals revealed the hexagonal structures of two new salts (Bi8)M[AlCl4]3 (M = Rb, Cs), which are isostructural to the high-temperature form of (Bi8)Tl[AlCl4]3. The known (Bi8)2+ polycation is a square antiprism and can be interpreted as an arachno cluster following modified Wade rules. The crystal structure is a complex variant of the hexagonal perovskite structure type ABX 3 with A = (Bi8)2+, B = M + and X = [AlCl4]–. Chiral strands ∞ { M [ AlCl 4 ] 3 } 2 − ∞ 1 $\infty {}_{\infty }{}^{1}{\left\{M{\left[{\text{AlCl}}_{4}\right]}_{3}\right\}}^{2-}$ (M = Rb, Cs) run along [001]. The (Bi8)2+ polycations are only weakly coordinated inside a cage of 24 chloride ions and show dynamic rotational disorder at room temperature. Upon slow cooling to 170 K, the reorientation of the clusters was frozen, yet no long-range order was established.

A Simple High-Yield Synthesis of Gallium(I) Tetrachlorogallate(III) and the Reaction of Digallium Tetrachloride Tetrahydrofuran Solvate with 1,2-Diols

2001 ◽  
Vol 56 (4-5) ◽  
pp. 337-341 ◽  
Author(s):  
Eva S. Schmidt ◽  
Annette Schier ◽  
Norbert W. Mitzel ◽  
Hubert Schmidbaur
Keyword(s):  
Crystalline Phase ◽  
Hydrogen Gas ◽  
High Yield ◽  
X Ray Diffraction ◽  
X Ray ◽  
Metal Atoms ◽  
Gallium Hydride ◽  
Hydroxy Groups ◽  
Tetrahydrofuran Solution ◽  
Analogous Product

Abstract Gallium(I) tetrachlorogallate(III) Ga[GaCU] was prepared in quantitative yield by thermal de­composition of dichlorogallane [HGaCl2]2, which is readily available from Et3SiH and [GaCl3]2. The reaction of catechol with solutions of this gallium(I) tetrachlorogallate(III) in tetrahydrofuran leads to the evolution of hydrogen gas and affords a dinuclear gallium(III) complex with penta-coordinate metal atoms chelated and bridged by mono-deprotonated catechol ligands. In the crystalline phase tetrahydrofuran molecules are hydrogen-bonded to the hydroxy groups: [Ga(1,2 -OC6H4OH)Cl2(C4H8O)]2. The reaction with pinacol also gives hydrogen and the analogous product [Ga(OCMe2CMe2OH)Cl2(C4H8O)]2. The structures of the two compounds have been determined by X-ray diffraction. A mechanism of the new reaction has been proposed which involves oxidative addition of the diol to the solvate (THF)Cl2Ga-GaCl2(THF) present in the tetrahydrofuran solution to give a gallium hydride intermediate.

STRUCTURAL AND ELECTROCHEMICAL PROPERTIES OF THIN LAYERS OF BINARY Ni–Fe ALLOYS ELECTRODEPOSITED BY TWO DIFFERENT BATHS: ACID AND IONIC LIQUID

2018 ◽  
Vol 25 (08) ◽  
pp. 1950025
Author(s):  
RAFIK MAIZI ◽  
ATHMANE MEDDOUR ◽  
CÉLINE ROUSSE
Keyword(s):  
Ionic Liquid ◽  
Nickel Content ◽  
Deposition Potential ◽  
Thin Layers ◽  
X Ray Diffraction ◽  
Sem Images ◽  
X Ray ◽  
Different Shapes ◽  
Fe Alloys ◽  
Irregular Behavior

The deposition of Ni–Fe thin layers in boric acid and ionic liquid ([BuMePyr][Tf2N]) baths were successfully prepared. The obtained materials have been characterized by X-ray diffraction (XRD), Energy Dispersive X-ray spectroscopy (EDX) and SEM. Meanwhile, these materials were carried out by chronoamperometry or chronopotentiometry by varying the intensity of the current and the deposition potential. The results indicate that the coatings of Ni–Fe alloys were successfully obtained by electroplating on the copper substrates, and the alloys composition shows irregular behavior with polarization. The nickel content in the samples is in the range of 55–90%, but the iron content ranges from 10–30%, when potential deposits were varied from [Formula: see text]2[Formula: see text]V to [Formula: see text]4[Formula: see text]V vs Ni electrode. The results also showed that the thin layers are monophased; they contain the Ni3Fe phase. Further, SEM images of Ni–Fe alloys show the different shapes of particles.

Improved Enzymatic Depolymerization of Chitosan by Ionic Liquid Pretreatment and the Effect of Oligo-Chitosan on Intestinal Flora In Vitro

2011 ◽  
Vol 391-392 ◽  
pp. 1319-1323
Author(s):  
Cui Zheng ◽  
Lin Li ◽  
Hao Pang ◽  
Zhao Mei Wang ◽  
Na Li
Keyword(s):  
Ionic Liquid ◽  
Hydrogen Bonds ◽  
Molecular Hydrogen ◽  
Intestinal Flora ◽  
X Ray Diffraction ◽  
X Ray ◽  
Hydrolysis Of ◽  
Positive Effect ◽  
Enzymatic Depolymerization

It still remains challenging for effective hydrolysis of chitosan into chitosan oligomers. In this work, a pretreatment was conducted on chitosan by an ionic liquid 1-butyl-3-methylimidazolium chloride ([C4mim]Cl), aiming at improving enzymatic depolymerization of chitosan. X-ray diffraction analysis indicated that the inter- and intra-molecular hydrogen bonds within chitosan molecules were broken by [C4mim]Cl and the crystalline was destroyed. The oligo-chitosan hydrolyzed from IL-pretreated chitosan, coded as COS-IL, showed a DP of 3~5, in contrast to DP 5~8 with oligo-chitosan obtained from untreated chitosan(coded as COS-UN). COS-IL was more effective than COS-UN in inhibiting intestinal spoilage bacterials growth and it has positive effect on the growth of intestinal probiotic bacterials.

Synthesis of Nickel Hydroxide with Different Morphologies Using an Ionic Liquid

2010 ◽  
Vol 663-665 ◽  
pp. 1163-1166
Author(s):  
Cun Ying Xu ◽  
Yi Xin Hua
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
Ionic Liquid ◽  
Volume Ratio ◽  
X Ray Diffraction ◽  
X Ray ◽  
Reaction Media ◽  
Solvothermal Conditions ◽  
Facile Route ◽  
Scanning Electron

A new and facile route has been developed to synthesize β-Ni(OH)2 nanostructures using ionic liquid 1-butyl-3-methylimidazolium tetrafluoroborate ([Bmim]BF4) as reaction media under solvothermal conditions. The β-Ni(OH)2 with different morphologies, such as nanoflakes, nanoplatelet and nanorods, can be obtained by controlling the volume ratio of the ionic liquid to water and reaction temperature. The as-prepared products were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM).

scholarly journals Preparation of Reswellable Amorphous Porous Celluloses through Hydrogelation from Ionic Liquid Solutions

Materials ◽  
2019 ◽  
Vol 12 (19) ◽  
pp. 3249 ◽  
Author(s):  
Satoshi Idenoue ◽  
Yoshitaka Oga ◽  
Daichi Hashimoto ◽  
Kazuya Yamamoto ◽  
Jun-ichi Kadokawa
Keyword(s):  
Mechanical Properties ◽  
Ionic Liquid ◽  
Amorphous Structure ◽  
X Ray Diffraction ◽  
Electron Microscopic ◽  
X Ray ◽  
Liquid Solutions ◽  
Scanning Electron Microscopic ◽  
Porous Morphology ◽  
Scanning Electron

In this study, we have performed the preparation of reswellable amorphous porous celluloses through regeneration from hydrogels. The cellulose hydrogels were first prepared from solutions with an ionic liquid, 1-butyl-3-methylimidazolium chloride (BMIMCl), in different concentrations. Lyophilization of the hydrogels efficiently produced the regenerated celluloses. The powder X-ray diffraction and scanning electron microscopic measurements of the products suggest an amorphous structure and porous morphology, respectively. Furthermore, the pore sizes of the regenerated celluloses, or in turn, the network sizes of cellulose chains in the hydrogels, were dependent on the concentrations of the initially prepared solutions with BMIMCl, which also affected the tensile mechanical properties. It was suggested that the dissolution states of the cellulose chains in the solutions were different, in accordance with the concentrations, which representatively dominated the pore and network sizes of the above materials. When the porous celluloses were immersed in water, reswelling was observed to regenerate the hydrogels.

scholarly journals Kristallchemische Analyse der Stereochemie des Kations und Anions in Bis(triphenylphosphin)iminium-di(phthalocyaninato)metallaten der Selenen Erden, (PNP)[Ln(Pc2-)2]•xH2O (Ln = La, Gd, Tm; x ≤ 0,5) / Crystalchemical analysis of the stereochemistry of the cations and anions in bis(triphenylphosphine)iminium di(phthalocyaninato)metalates of the rare earth elements, (PNP)[Ln(Pc2-)2]•xH2O (Ln = La, Gd, Tm; x ≤ 0,5)

1994 ◽  
Vol 49 (6) ◽  
pp. 812-820 ◽  
Author(s):  
Mohsen Safarpour Haghighi ◽  
Andreas Franken ◽  
Heiner Homborg
Keyword(s):  
Structural Characteristics ◽  
Steric Effects ◽  
X Ray Diffraction ◽  
X Ray ◽  
Contact Distance ◽  
The Common ◽  
Complex Salts ◽  
Cell Data ◽  
Unit Cell Data ◽  
Ir Bands

Of the isostructural series of monoclinic (PNP)[Ln(Pc)2]• xH2O compounds (Ln = La ••• Tm) the crystal structures of the complex salts of tervalent La (1), Gd (2) and Tm (3) have been determined by single crystal X-ray diffraction analysis. Unit cell data for 2: space group P21/c; a = 15.172(8), b = 20.826(2), c = 25.876(3) Å, β = 95.19(3)°, V - 8143(4) Å3, Z = 4; 1 and 3 are isostructural with 2. The lanthanide ion occupies the center of a nearly ideal square antiprism, although the two staggered phthalocyanine rings are severely distorted in an unsymmetrical funnel-shaped fashion due to electronic, steric, and packing influences in the crystal lattice. Steric effects dictate also the geometry of the PNP cation, which adopts a hybrid conformation whose structural characteristics are between the common linear and bent conformers with medium short P-N distances (1.562 Å) and large P-N-P angles in the range 165.6° (1) > 158.3° (2) > 156.1° (3). The strong IR bands at ca. 1375 cm-1 assigned to the asym. (P-N) stretch are diagnostic for this hybrid conformation. The presence of water of crystallization in the periphery of the diphthalocyanine anion is confirmed. The shortest contact distance is observed to one of the bridging nitrogen atoms of the Pc2- ligand (3.02 Å) indicating a weak (HO-H•••N) hydrogen bond

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