scholarly journals Bulking up CpBIG: A Penta-Terphenyl Cyclopentadienyl Ligand

2022 ◽  
Author(s):  
Gabriele Hierlmeier ◽  
Robert Wolf
Keyword(s):  
Metal Salts ◽  
Formula Unit ◽  
Alkali Metal Salts ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cyclopentadienyl Ligand ◽  
Vis Spectroscopy ◽  
Multinuclear Nmr Spectroscopy ◽  
Complete Series ◽  
Group 1

The modification of cyclopentadienyl ligands with carefully selected substituents is a widely used strategy to tune their steric and electronic properties. We describe the synthesis of an extremely bulky penta-terphenyl cyclopentadienyl ligand (CpT5) by arylation of cyclopentadiene. Deprotonation reactions with various group 1 metals and bases afforded a complete series of alkali metal salts MCpT5 with M = Li to Cs. The compounds were isolated as solvate-free salts, which were characterized by multinuclear NMR spectroscopy, UV-vis spectroscopy and elemental analysis. Single-crystal X-ray diffraction studies on LiCpT5, NaCpT5 (crystallized as a solvate with one THF molecule per formula unit) and KCpT5 revealed the formation of metallocene-like sandwich structures in the solid state.

Unexpected lyotropic liquid crystals from ion-induced columnar assembly of Schiff-base macrocycles

2012 ◽  
Vol 90 (12) ◽  
pp. 1056-1062 ◽  
Author(s):  
Joseph K.-H. Hui ◽  
Jian Jiang ◽  
Mark J. MacLachlan
Keyword(s):  
Electron Microscopy ◽  
Schiff Base ◽  
Liquid Crystals ◽  
Lyotropic Liquid Crystals ◽  
Metal Salts ◽  
Alkali Metal Salts ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Schiff Base Macrocycles

Schiff-base macrocycles 1, which have a crown ether-like interior, form ionic nematic lyotropic liquid crystals in various organic solvents when functionalized with long alkoxy substituents and complexed to diverse ammonium and alkali metal salts. From X-ray diffraction and transmission electron microscopy studies, and by comparison with the organization of macrocycles functionalized with shorter chains, these macrocycles assemble into lyotropic liquid crystals where the macrocycles are stacked and the cation is included in their interiors.

scholarly journals Metal Complexes of π-expanded Ligand (5): Synthesis, Structural, and Photophysical Characterizations of Green-Red Luminescent Pyrene-based Salicylaldiminato-type Zinc Complexes

2021 ◽  
Vol 37 (2) ◽  
Author(s):  
Luong Xuan Dien ◽  
Nguyen Thi Thuy Nga
Keyword(s):  
Sodium Acetate ◽  
Density Functional ◽  
Emission Spectra ◽  
Molecular Orbital Calculations ◽  
X Ray Diffraction ◽  
Functional Theory ◽  
X Ray ◽  
Imine Nitrogen ◽  
Vis Spectroscopy ◽  
Group 1

A series of pyrene-based salicylaldimine-type ligands containing n-octyl or cyclohexyl or phenyl groups at imine nitrogen group, 1-hydroxy-2-[(N-substituted-imino)methyl]-pyrenes (octyl 1, cyclohexyl 1b and phenyl 1c), were synthesized and characterized. The ligands reacting with zinc acetate in the presence of sodium acetate gave the bis(salicylaldiminato)-type Zn(II) complexes, [bis[2-[(N-substituted-imino)methyl]-1-pyrenolato-N,O] zinc(II)] (octyl 1(Zn), cyclohexyl 1b(Zn), phenyl 1c(Zn)). The new ligands and complexes were characterized by 1H NMR, IR spectroscopy, mass spectroscopy, elemental analysis, UV-vis spectroscopy, fluorescence spectroscopy, and X-ray diffraction. The influence of the π-extended conjugation of the pyrene-based salicylaldiminato-type ligands coordinated to Zn2+ greatly induces red-shift of the complexes 1(Zn), 1b(Zn) and 1c(Zn) in absorption and emission spectra. These results were confirmed by density-functional theory (DFT) and time-dependent DFT (TDDFT) molecular orbital calculations. Moreover, single crystal structure of simple salicylaldiminato Zn(II) complex 1’b(Zn) was compared to that of the corresponding pyrene-type salicylaldiminato complex 1b(Zn).

Effect of Hydrated Metal Salts on the Coordination Product of Cobalt(II) halide and PNP Type Ligand, 2,6-bis(di-tertbutylphosphinomethyl) pyridine

2018 ◽  
Author(s):  
Tasneem Siddiquee ◽  
Abdul Goni
Keyword(s):  
Metal Salts ◽  
Molar Ratio ◽  
Pincer Complexes ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
Pincer Ligand ◽  
Tetrahedral Geometry ◽  
X Ray ◽  
Distorted Tetrahedral Geometry ◽  
Cobalt Center

Chemical treatment of CoX<sub>2</sub><b><sup>. </sup></b>6H<sub>2</sub>O (X = Cl, Br, I) with the potentially tridentate PNP pincer ligand 2,6-bis(di-<i>tert</i>-butylphosphinomethyl)pyridine in 1:1 molar ratio results in cobalt(II) halide-PNP pincer complexes. The effect of the hydrated metal source on molecular structure and geometry of the complexes was studied by single crystal X-ray diffraction analysis. The complexes are neutral and the cobalt center adopts a penta-coordinate system with potential atropisomerization. Within the unit cell there are two distinct molecules per asymmetric unit. One of the two phosphorus atoms in the PNP ligand was observed to be partially oxidized to phosphinoxide. Disorder in the structure reflects a mixture of square pyramidal and distorted tetrahedral geometry.

Unusual Rearrangement of Naphthalene in the Synthesis of a Novel B8-B8-Bridged Derivative in the [(1,2-C2B9H11)2-3-Co]- Series. X-Ray Structure and 11B NMR Spectra of [8,8'-μ-(CH2-C9H6)-(1,2-C2B9H10)2-3-Co]- (CH3)4N+

1997 ◽  
Vol 62 (5) ◽  
pp. 746-751 ◽  
Author(s):  
Andreas Franken ◽  
Jaromír Plešek ◽  
Christiane Nachtigal
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Nucleophilic Substitution ◽  
Nmr Spectra ◽  
X Ray Diffraction ◽  
X Ray ◽  
Unusual Rearrangement ◽  
Multinuclear Nmr Spectroscopy ◽  
11B Nmr ◽  
Isolated Compound

On treatment of the [(1,2-C2B9H11)2Co]- ion with naphthalene in presence of AlCl3 a remarkably bridged [8,8'-μ-(CH2-C9H6)-(1,2-C2B9H10)2-3-Co]- ion is obtained as a single isolated compound. The triatomic -CH2-C9H6- bridge is derived from the rearranged naphthalene nucleus. The mechanism of this reaction is obscure but it does resemble the "Electrophile-Induced Nucleophilic Substitution" reported earlier. The structure of the compound was established by multinuclear NMR spectroscopy and by single crystal X-ray diffraction.

Nanocrystalline Solutions as Precursors to The Spray Deposition of Cdte Thin Films

1995 ◽  
Vol 382 ◽  
Author(s):  
Martin Pehnt ◽  
Douglas L. Schulz ◽  
Calvin J. Curtis ◽  
Helio R. Moutinho ◽  
Amy Swartzlander ◽  
...  
Keyword(s):  
Thin Films ◽  
Atomic Force Microscopy ◽  
Grain Size ◽  
X Ray Diffraction ◽  
X Ray ◽  
Force Microscopy ◽  
Cdte Nanoparticles ◽  
Atomic Force ◽  
Vis Spectroscopy ◽  
Cdte Thin Films

ABSTRACTIn this article we report the first nanoparticle-derived route to smooth, dense, phase-pure CdTe thin films. Capped CdTe nanoparticles were prepared by injection of a mixture of Cd(CH3)2, (n-C8H17)3 PTe and (n-C8H17)3P into (n-C8H17)3PO at elevated temperatures. The resultant nanoparticles 32-45 Å in diameter were characterized by x-ray diffraction, UV-Vis spectroscopy, transmission electron microscopy, thermogravimetric analysis and energy dispersive x-ray spectroscopy. CdTe thin film deposition was accomplished by dissolving CdTe nanoparticles in butanol and then spraying the solution onto SnO2-coated glass substrates at variable susceptor temperatures. Smooth and dense CdTe thin films were obtained using growth temperatures approximately 200 °C less than conventional spray pyrolysis approaches. CdTe films were characterized by x-ray diffraction, UV-Vis spectroscopy, atomic force microscopy, and Auger electron spectroscopy. An increase in crystallinity and average grain size as determined by x-ray diffraction was noted as growth temperature was increased from 240 to 300 °C. This temperature dependence of film grain size was further confirmed by atomic force microscopy with no remnant nanocrystalline morphological features detected. UV-Vis characterization of the CdTe thin films revealed a gradual decrease of the band gap (i.e., elimination of nanocrystalline CdTe phase) as the growth temperature was increased with bulk CdTe optical properties observed for films grown at 300 °C.

Salts of purine alkaloids caffeine and theobromine with 2,6-dihydroxybenzoic acid as coformer: structural, theoretical, thermal and spectroscopic studies

2021 ◽  
Vol 77 (11) ◽  
Author(s):  
Mateusz Gołdyn ◽  
Anna Komasa ◽  
Mateusz Pawlaczyk ◽  
Aneta Lewandowska ◽  
Elżbieta Bartoszak-Adamska
Keyword(s):  
Hydrogen Bonds ◽  
Water Solubility ◽  
Theoretical Calculations ◽  
Spectroscopic Studies ◽  
X Ray Diffraction ◽  
Dihydroxybenzoic Acid ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Purine Alkaloids ◽  
Vis Spectroscopy

The study of various forms of pharmaceutical substances with specific physicochemical properties suitable for putting them on the market is one of the elements of research in the pharmaceutical industry. A large proportion of active pharmaceutical ingredients (APIs) occur in the salt form. The use of an acidic coformer with a given structure and a suitable pK a value towards purine alkaloids containing a basic imidazole N atom can lead to salt formation. In this work, 2,6-dihydroxybenzoic acid (26DHBA) was used for cocrystallization of theobromine (TBR) and caffeine (CAF). Two novel salts, namely, theobrominium 2,6-dihydroxybenzoate, C7H9N4O2 +·C7H5O4 − (I), and caffeinium 2,6-dihydroxybenzoate, C8H11N4O2 +·C7H5O4 − (II), were synthesized. Both salts were obtained independently by slow evaporation from solution, by neat grinding and also by microwave-assisted slurry cocrystallization. Powder X-ray diffraction measurements proved the formation of the new substances. Single-crystal X-ray diffraction studies confirmed proton transfer between the given alkaloid and 26DHBA, and the formation of N—H...O hydrogen bonds in both I and II. Unlike the caffeine cations in II, the theobromine cations in I are paired by noncovalent N—H...O=C interactions and a cyclic array is observed. As expected, the two hydroxy groups in the 26DHBA anion in both salts are involved in two intramolecular O—H...O hydrogen bonds. C—H...O and π–π interactions further stabilize the crystal structures of both compounds. Steady-state UV–Vis spectroscopy showed changes in the water solubility of xanthines after ionizable complex formation. The obtained salts I and II were also characterized by theoretical calculations, Fourier-transform IR spectroscopy (FT–IR), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) and elemental analysis.

scholarly journals Thermal and optical properties of new poly(amide-imide)-nanocomposite reinforced by layer silicate based on chiral n-trimellitylimido-L-valine

2012 ◽  
Vol 31 (1) ◽  
pp. 79
Author(s):  
Khalil Faghihi ◽  
Masoumeh Soleimani ◽  
Shabnam Nezami ◽  
Meisam Shabanian
Keyword(s):  
Main Chain ◽  
Nanocomposite Films ◽  
Direct Polycondensation ◽  
Polycondensation Reaction ◽  
X Ray Diffraction ◽  
Solution Intercalation ◽  
X Ray ◽  
Vis Spectroscopy ◽  
Polymeric Chains ◽  
Morphology And Structure

Two new samples of poly(amide-imide)-montmorillonite reinforced nanocomposites containing N-trimellitylimido-L-valine moiety in the main chain were synthesized by a convenient solution intercalation technique. Poly(amide-imide) (PAI) 5 as a source of polymer matrix was synthesized by the direct polycondensation reaction of N-trimellitylimido-L-valine (3) with 4,4′-diaminodiphenyl ether 4 in the presence of triphenyl phosphite (TPP), CaCl2, pyridine and N-methyl-2-pyrrolidone (NMP). Morphology and structure of the resulting PA-nanocomposite films (5a) and (5b) with 10 and 20 % silicate particles were characterized by FTIR spectroscopy, X-ray diffraction (XRD) and scanning electron microscopy (SEM). The effect of clay dispersion and the interaction between clay and polymeric chains on the properties of nanocomposite films were investigated by using Uv-vis spectroscopy,  thermogravimetric analysis (TGA) and water uptake measurements.

scholarly journals A Covalent Organic Cage Compound Acting as a Supramolecular Shadow Mask for the Regioselective Functionalization of C60

2020 ◽  
Author(s):  
Viktoria Leonhardt ◽  
Stefanie Fimmel ◽  
Ana-Maria Krause ◽  
Florian Beuerle
Keyword(s):  
Mass Spectrometry ◽  
Single Crystal ◽  
High Selectivity ◽  
Shadow Mask ◽  
X Ray Diffraction ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Cage Compound ◽  
Vis Spectroscopy ◽  
Regioselective Functionalization

<div><div><div><p>A trigonal-bipyramidal covalent organic cage compound serves as an efficient host to form stable 1:1-complexes with C60 and C70. Fullerene encapsulation has been comprehensively studied by NMR and UV/Vis spectroscopy, mass spectrometry as well as single-crystal X-ray diffraction. Exohedral functionalization of encapsulated C60 via threefold Prato reaction revealed high selectivity for the symmetry-matched all-trans-3 addition pattern.</p></div></div></div>

scholarly journals Caulerpa sertularioides extract as a complexing agent in the synthesis of ZnO and Zn(OH)2 nanoparticles and its effect in the azo dye’s photocatalysis in water

BioResources ◽  
2021 ◽  
Vol 16 (1) ◽  
pp. 1548-1560
Author(s):  
Daniel Garcia-Bedoya ◽  
Luis P. Ramírez-Rodríguez ◽  
Jesús M. Quiroz-Castillo ◽  
Edgard Esquer-Miranda ◽  
Arnulfo Castellanos-Moreno
Keyword(s):  
Azo Dyes ◽  
Industrial Wastewater ◽  
Methanol Extract ◽  
Complexing Agent ◽  
X Ray Diffraction ◽  
X Ray ◽  
Environmental Consequences ◽  
Photocatalytic Effect ◽  
Transmission Electron ◽  
Vis Spectroscopy

Algae constitute a diverse group that is useful in many biotechnological areas. In this paper, the usefulness of Caulerpa sertularioides methanol extract in the synthesis of ZnO and Zn(OH)2 nanoparticles was explored. This work had two main objectives: (1) to use the extract in the synthesis as an organic harmless complexing agent, and (2) to enhance a photocatalytic effect over AZO dyes in wastewater from fabric industries without adding nanomaterial to the environment due to its toxicity. Caulerpa extract performed the expected complexing action, and nanoparticles were formed in a size range from 45 to 69 nm. X-ray diffraction analysis (XRD), transmission electron microscopy (TEM) and UV-Vis spectroscopy were used to characterize the system. It was demonstrated that the nanoparticles were useful to photocatalyst AZO dyes in the water, while contained in tetraethylorthosilicate composites. These could be used in industrial wastewater and are expected to have no environmental consequences because the composites do not add nanoparticles to the water.

Sign in / Sign up

Export Citation Format

Share Document