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 ◽  
...  

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.

2015 ◽  
Vol 39 (10) ◽  
pp. 7595-7601 ◽  
Author(s):  
Farid M. Sroor ◽  
Cristian G. Hrib ◽  
Liane Hilfert ◽  
Sabine Busse ◽  
Frank T. Edelmann

New unsolvated, homoleptic lanthanide(iii) tris(cyclopropylethinylamidinate) complexes of the type [c-C3H5–CC–C(NR)2]3Ln (R = iPr, cyclohexyl; Ln = Nd, Sm, Ho) have been prepared and the crystal structure of the holmium derivative [c-C3H5–CC–C(NiPr)2]3Ho has been confirmed by X-ray diffraction.


2016 ◽  
Vol 18 (48) ◽  
pp. 32723-32734 ◽  
Author(s):  
Kaixin Li ◽  
Yibo Yan ◽  
Jun Zhao ◽  
Junxi Lei ◽  
Xinli Jia ◽  
...  

The intra- and inter-hydrogen bonding networks that govern the catalytic activity of Brønsted acidic ionic liquids were identified.


1994 ◽  
Vol 47 (7) ◽  
pp. 1401 ◽  
Author(s):  
DE Lynch ◽  
G Smith ◽  
KA Byriel ◽  
CHL Kennard ◽  
AK Whittaker ◽  
...  

A series of 1:1 molecular adducts of triphenylphosphine oxide ( tppo ) with substituted phenoxyacetic acids has been prepared and characterized by using infrared, solid-state 1H and 31P n.m.r. spectroscopy, and X-ray powder diffraction methods. The crystal structure of one of these, with the herbicidally active (4-chloro-2-methylphenoxy)acetic acid ( mcpa ),[( tppo )( mcpa )], has been determined by X-ray diffraction methods. This compound is isomorphous with the tppo adduct of (2,4-dichlorophenoxy)acetic acid. The title compound has two independent and different molecular adducts in the asymmetric unit each with strong hydrogen-bonding interactions between the carboxylic acid proton and the phosphoryl oxygen of tppo [O...O, 2.579, 2.647(9)Ǻ].


1995 ◽  
Vol 48 (4) ◽  
pp. 869 ◽  
Author(s):  
G Smith ◽  
EJ Oreilly ◽  
SA See ◽  
KA Byriel ◽  
CHL Kennard

The ring-substituted phenoxyacetic acid (2-benzoyl-5-methoxyphenoxy)acetic acid (HL) (3) and its complex adduct dimer (4) with sodium, [Na2(L)2(HL)2].2HL, have been synthesized and their structures determined by X-ray diffraction. The acid (3) does not have the usual cyclic hydrogen-bonded dimer association, but instead has three-centre intramolecular hydrogen bonding between the carboxyl proton and both the ether and keto oxygens [O---O, 2.602(3), 2.711(3) Ǻ respectively]. Each sodium in the centrosymmetric complex dimer (4) is seven-coordinate [Na-O, 2.313(5)-2.612(5) Ǻ], involving the 'inner' three oxygens of both a protonated and an ionic ligand molecule. In addition, one of these carboxyl oxygens forms a bridge to the inversion-related sodium, while the uncoordinated carboxyl oxygen is hydrogen-bonded to a protonated carboxy group [O---O, 2.464(8) Ǻ]. The molecules of the lattice acid have only one hydrogen-bonded association with the second uncoordinated carboxy group in the dimer [O---O, 2.513(7) Ǻ].


2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Maximilian Knies ◽  
Michael Ruck

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.


2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Maximilian Knies ◽  
Michael Ruck

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.


2021 ◽  
Vol 16 (2) ◽  
pp. 260-266
Author(s):  
Li-Hua Wang ◽  
Fan-Yuan Kong ◽  
Xi-Shi Tai

A new six-coordinated Mn(II) coordination polymer, [Mn(L1)(L2)2]n (L1 = 2-aminopyrimidine, HL2 = 3-bromo-2-hydroxybenzaldehyde) was synthesized by 3-bromo-2-hydroxybenzaldehyde, NaOH, 2-aminopyrimidine and manganese(II) acetate dihydrate. The Mn(II) coordination polymer was structural characterized by elemental analysis and single crystal X-ray diffraction. The results show that each Mn(II) ion is six-coordinated with two phenolic hydroxyl O atoms from two 3-bromo-2-hydroxybenzaldehyde ligands (O1 and O4), two formyl group O atoms from two 3-bromo-2-hydroxybenzaldehyde ligands (O2 and O3), and two N atoms from two 2-aminopyrimidine molecules (N1A and N2), and forms a distorted octahedral coordination geometry. The Mn(II) coordination polymer displays a 1D chained structure by the bridge effect of 2-aminopyrimidine N atoms. The catalytic activities of Mn(II) coordination polymer and Pd@Mn(II) coordination polymer for hydrogenation of 1,3-butadiene have been investigated. The Pd@Mn(II) coordination polymer catalyst shows the good catalytic activity and selectivity in  the hydrogenation of 1,3-butadiene. The 1,3-butadiene conversion is 61.3% at 70 °C, and the selectivity to total butene is close to 100%. Copyright © 2021 by Authors, Published by BCREC Group. This is an open access article under the CC BY-SA License (https://creativecommons.org/licenses/by-sa/4.0). 


2014 ◽  
Vol 983 ◽  
pp. 20-25 ◽  
Author(s):  
Yu He Cheng ◽  
Biao Zhang ◽  
Shang Jiang Dai ◽  
Han Lin Tong ◽  
Li Xia Li

A series of polystyrene-supported 1-(propyl-3-sulfonate)-3-methy-imidazolium hydrosulfate acidic ionic liquid (PS-[SO3H-PMIM][HSO4]) catalysts with different [SO3H-PMIM][HSO4] contents were prepared and tested for esterification of n-butyl alcohol with acetic acid. It was found that the reactivity of the catalyst increased with increasing [SO3H-PMIM][HSO4] content, and best yield of n-Butyl acetate of 98% was obtained using PS-[SO3H-PMIM][HSO4]1 within 1.5h. The catalytic activity of this catalyst decreased slightly after fifth using.


2014 ◽  
Vol 955-959 ◽  
pp. 62-65 ◽  
Author(s):  
Peng Hui Shi ◽  
Hon Gai Zheng ◽  
Wei Feng Yao ◽  
Qiang Wu ◽  
Si Yu Tan ◽  
...  

A variety of loadings of Cobalt oxide (Co3O4) was successfully supported on the reduced graphene (Co3O4/rGO) as the catalyst to activate peroxymonosulfate (PMS) to generate sulfate radicals (SO4−•) for degrading Orange II in water. The crystal structure of Co3O4/rGO with different loadings was characterized by X-ray diffraction (XRD), and their catalytic activity was compared in the same conditions. The result showed that the catalyst has an optimum Co3O4 loading. Using the 70.7% loading of Co3O4 in Co3O4/rGO as the catalyst, 100% decomposition could be achieved within 4 min with 1 mM Orange II, 0.05g/L catalyst, and 10 mM PMS.


1980 ◽  
Vol 33 (8) ◽  
pp. 1847 ◽  
Author(s):  
DL Kepert ◽  
BW Skelton ◽  
AH White

The crystal structure of the title compound, Mo2(O2CCH3)4,Na+ - O2CCH3,HO2CCH3, has been determined by single crystal X-ray diffraction at 295(1) K and refined by least squares to a residual of 0.040 for 1529 'observed' reflections. Crystals are monoclinic, space group I2/c, a 8.251(5), b 18.468(9), c 13.674(6) Ǻ, β 100.25(4)°, Z 4. The compound is shown to have the above stoichiometry, containing the usual binuclear molybdenum(II) acetate cluster together with pairs of hydrogen-bonded acetic acid/acetate units.


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