scholarly journals Coordination-driven self-assembly of discrete Ru6–Pt6 prismatic cages

2018 ◽  
Vol 14 ◽  
pp. 2242-2249 ◽  
Author(s):  
Aderonke Ajibola Adeyemo ◽  
Partha Sarathi Mukherjee
Keyword(s):  
Mass Spectrometry ◽  
Self Assembly ◽  
Room Temperature ◽  
Geometry Optimization ◽  
Platinum Metal ◽  
Major Product ◽  
Spectroscopic Techniques ◽  
One Pot ◽  
Infrared Studies ◽  
Trigonal Prismatic

The coordination-driven self-assembly of two new Ru6–Pt6 hexanuclear trigonal prismatic cages comprising arene–ruthenium(II) clips (1a(NO 3 ) 2 and 1b(NO 3 ) 2 ) and a tritopic platinum(II) metalloligand 2 has been performed in methanol at room temperature. The [3 + 2] hexanuclear cages 3a and 3b were isolated in good yields and characterized by well-known spectroscopic techniques including multinuclear NMR, mass spectrometry, UV–vis and infrared studies. Geometry optimization revealed the shapes and sizes of these hexanuclear prismatic cages. The combination of ruthenium and platinum metal center in a one-pot self-assembly reaction showcases the construction of aesthetically elegant heterometallic structures in supramolecular chemistry leading to the formation of a single major product.

Click Synthesis of Shape-Persistent Azodendrimers and their Orthogonal Self-Assembly to Nanofibres

2018 ◽  
Vol 71 (6) ◽  
pp. 463 ◽  
Author(s):  
Tamer El Malah ◽  
Hany F. Nour
Keyword(s):  
Electron Microscopy ◽  
Mass Spectrometry ◽  
Self Assembly ◽  
Molecular Structures ◽  
Side Chain ◽  
Spectroscopic Techniques ◽  
Molecular Weights ◽  
Transmission Electron ◽  
Click Synthesis ◽  
Scanning Electron

The copper(i)-catalyzed azide–alkyne cycloaddition (CuAAC) reaction has been efficiently utilized to synthesize a series of dendrons with amino functionalities. The aminodendrons successfully underwent azodimerization to furnish a series of pyridyl- and phenyl-based azodendrimers with peripheral alkyl or ether side chain substituents. The molecular structures of the azodendrimers were fully assigned using different spectroscopic techniques, such as 1H NMR and 13C NMR, and the molecular weights were determined using MALDI-TOF mass spectrometry. The molecular self-assembly of the azodendrimers was investigated by scanning electron microscopy and transmission electron microscopy, which revealed the formation of highly ordered and uniform self-assembled nanofibres.

Synthesis, photoinduced amination and topological indices of novel porphyrin dyads

2020 ◽  
Vol 24 (08) ◽  
pp. 1054-1065
Author(s):  
Muhammad Yaseen ◽  
Muhammad A. Rashid ◽  
Muhammad A. Iqbal ◽  
Zahid Farooq ◽  
Muhammad Idrees ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Transition Metal ◽  
Elemental Analysis ◽  
Room Temperature ◽  
Topological Indices ◽  
Operational Cost ◽  
One Pot ◽  
H Nmr ◽  
Metal Catalyzed ◽  
The One

Transition-metal-catalyzed homo and hetero coupling is a rapidly growing area of research. This work refers to the nickel-catalyzed photoinduced amination study of [Formula: see text]-bromotetraarylporphyrin and its Ni(II), Zn(II) and Cu(II) complexes. The selective mono [Formula: see text]-bromination of 5,10,15,20-tetrakis(4[Formula: see text]-isopropylphenyl)porphyrin was achieved with [Formula: see text]-bromosuccinimide. Under similar conditions, [Formula: see text]-bromination of Ni(II), Zn(II) and Cu(II) complexes of 5,10,15,20-tetrakis(4[Formula: see text]-isopropylphenyl)porphyrin successfully afforded the corresponding 2-bromometalloporphyrins. The [Formula: see text]-bromoporphyrin/metalloporphyrins were coupled with three different amines through the creation of the C–N bond by using an economical and air-tolerant photoactive catalyst (NiBr[Formula: see text] · 3H2O) at room temperature under 365 nm radiations. Nickel-catalyzed amination yields are compared with the traditional Buchwald–Hartwig amination yields. Due to the low operational cost, photoinduced nickel-catalyzed C–N couplings were found to be more economical than the Buchwald–Hartwig amination procedure, although the latter afforded higher yields. The nickel-catalyzed photoamination reaction was also extended for the one-pot synthesis of pyridine-3,5-diamine bridged porphyrin dyad. The intramolecular cyclization of the pyridine-3,5-diamine-bridged porphyrin dyad afforded a novel quinolino-fused porphyrin dyad. Degree- and distance-based topological indices of the newly synthesized porphyrins were calculated and correlated with their molar refractivity. All newly synthesized porphyrins are characterized by UV-vis, FTIR, 1H NMR, elemental analysis and mass spectrometry.

scholarly journals Controlling the Shape and Chirality of an Eight-crossing Molecular Knot

2020 ◽  
Author(s):  
John P. Carpenter ◽  
Charlie McTernan ◽  
Jake L. Greenfield ◽  
Roy Lavendomme ◽  
Tanya K. Ronson ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Self Assembly ◽  
Metal Salt ◽  
Molecular Machines ◽  
One Pot ◽  
X Ray ◽  
X Ray Crystallography ◽  
And Topology ◽  
Simple Pair ◽  
And Control

<p>The knotting of biomolecules impacts their function, and enables them to carry out new tasks. Likewise, complex topologies underpin the operation of many synthetic molecular machines. The ability to generate and control more complex knotted architectures is essential to endow these machines with more advanced functions. Here we report the synthesis of a molecular knot with eight crossing points, consisting of a single organic loop woven about six templating metal centres, <i>via</i> one-pot self-assembly from a simple pair of dialdehyde and diamine subcomponents and a single metal salt. The structure and topology of the knot were established by NMR spectroscopy, mass spectrometry and X-ray crystallography. Upon demetallation, the purely organic strand relaxes into a symmetric conformation, whilst retaining the topology of the original knot. This knot is topologically chiral, and may be synthesised diastereoselectively through the use of an enantiopure diamine building block.<b></b></p>

scholarly journals Controlling the Shape and Chirality of an Eight-crossing Molecular Knot

2020 ◽  
Author(s):  
John P. Carpenter ◽  
Charlie McTernan ◽  
Jake L. Greenfield ◽  
Roy Lavendomme ◽  
Tanya K. Ronson ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Self Assembly ◽  
Metal Salt ◽  
Molecular Machines ◽  
One Pot ◽  
X Ray ◽  
X Ray Crystallography ◽  
And Topology ◽  
Simple Pair ◽  
And Control

<p>The knotting of biomolecules impacts their function, and enables them to carry out new tasks. Likewise, complex topologies underpin the operation of many synthetic molecular machines. The ability to generate and control more complex knotted architectures is essential to endow these machines with more advanced functions. Here we report the synthesis of a molecular knot with eight crossing points, consisting of a single organic loop woven about six templating metal centres, <i>via</i> one-pot self-assembly from a simple pair of dialdehyde and diamine subcomponents and a single metal salt. The structure and topology of the knot were established by NMR spectroscopy, mass spectrometry and X-ray crystallography. Upon demetallation, the purely organic strand relaxes into a symmetric conformation, whilst retaining the topology of the original knot. This knot is topologically chiral, and may be synthesised diastereoselectively through the use of an enantiopure diamine building block.<b></b></p>

scholarly journals On the fly multi-modal observation of ligand synthesis and complexation of Cu complexes in flow with ‘benchtop’ NMR and mass spectrometry

2016 ◽  
Vol 3 (7) ◽  
pp. 919-923 ◽  
Author(s):  
Luzian Porwol ◽  
Alon Henson ◽  
Philip J. Kitson ◽  
De-Liang Long ◽  
Leroy Cronin
Keyword(s):  
Mass Spectrometry ◽  
Real Time ◽  
Self Assembly ◽  
Coordination Compounds ◽  
The Self ◽  
One Pot ◽  
Time Observation ◽  
Set Up ◽  
Cu Complexes ◽  
Real Time Observation

The transfer of one-pot reactions to a continuous non-equilibrium set-up for real-time observation of the self-assembly of new coordination compounds is presented.

Characterization of intergranular cuprous oxide in polycrystalline YBa2Cu3O7-x

1988 ◽  
Vol 46 ◽  
pp. 880-881
Author(s):  
Bradley L. Thiel ◽  
Chan Han R. P. ◽  
Kurosky L. C. Hutter ◽  
I. A. Aksay ◽  
Mehmet Sarikaya
Keyword(s):  
Grain Boundary ◽  
Cuprous Oxide ◽  
Room Temperature ◽  
Boundary Phase ◽  
Spectroscopic Techniques ◽  
Transition Width ◽  
Practical Applications ◽  
Thin Foils ◽  
Superconducting Oxides

The identification of extraneous phases is important in understanding of high Tc superconducting oxides. The spectroscopic techniques commonly used in determining the origin of superconductivity (such as RAMAN, XPS, AES, and EXAFS) are surface-sensitive. Hence a grain boundary phase several nanometers thick could produce irrelevant spectroscopic results and cause erroneous conclusions. The intergranular phases present a major technological consideration for practical applications. In this communication we report the identification of a Cu2O grain boundary phase which forms during the sintering of YBa2Cu3O7-x (1:2:3 compound).Samples are prepared using a mixture of Y2O3. CuO, and BaO2 powders dispersed in ethanol for complete mixing. The pellets pressed at 20,000 psi are heated to 950°C at a rate of 5°C per min, held for 1 hr, and cooled at 1°C per min to room temperature. The samples show a Tc of 91K with a transition width of 2K. In order to prevent damage, a low temperature stage is used in milling to prepare thin foils which are then observed, using a liquid nitrogen holder, in a Philips 430T at 300 kV.

Green synthesis of mixed metallic nanoparticles using room temperature self-assembly

2017 ◽  
Vol 13 (2) ◽  
pp. 4671-4677 ◽  
Author(s):  
A. M. Abdelghany ◽  
A.H. Oraby ◽  
Awatif A Hindi ◽  
Doaa M El-Nagar ◽  
Fathia S Alhakami
Keyword(s):  
Self Assembly ◽  
Metallic Nanoparticles ◽  
Room Temperature ◽  
Bimetallic Nanoparticles ◽  
Reduction Process ◽  
Nano Particles ◽  
Nano Structure ◽  
Small Shift ◽  
Molar Ratios ◽  
Vis Spectroscopy

Bimetallic nanoparticles of silver (Ag) and gold (Au) were synthesized at room temperature using Curcumin. Reduction process of silver and gold ions with different molar ratios leads to production of different nanostructures including alloys and core-shells. Produced nanoparticles were characterized simultaneously with FTIR, UV/vis. spectroscopy, transmission electron microscopy (TEM), and Energy-dispersive X-ray (EDAX). UV/vis. optical absorption spectra of as synthesized nanoparticles reveals presence of surface palsmon resonance (SPR) of both silver at (425 nm) and gold at (540 nm) with small shift and broadness of gold band after mixing with resucing and capping agent in natural extract which suggest presence of bimetallic nano structure (Au/Ag). FTIR and EDAX data approve the presence of bimetallic nano structure combined with curcumin extract. TEM micrographs shows that silver and gold can be synthesized separately in the form of nano particles using curcumin extract. Synthesis of gold nano particles in presence of silver effectively enhance and control formation of bi-metallic structure.

Room Temperature Alkali Metal Reduction of Carbon Dioxide

2020 ◽  
Author(s):  
Lucas A. Freeman ◽  
Akachukwu D. Obi ◽  
Haleigh R. Machost ◽  
Andrew Molino ◽  
Asa W. Nichols ◽  
...  
Keyword(s):  
Alkali Metal ◽  
Alkali Metals ◽  
Room Temperature ◽  
Chemical Reduction ◽  
Bond Cleavage ◽  
Open Shell ◽  
Metal Reduction ◽  
One Pot ◽  
Earth Abundant ◽  
Electron Reduction

The reduction of the relatively inert carbon–oxygen bonds of CO<sub>2</sub> to access useful CO<sub>2</sub>-derived organic products is one of the most important fundamental challenges in synthetic chemistry. Facilitating this bond-cleavage using earth-abundant, non-toxic main group elements (MGEs) is especially arduous because of the difficulty in achieving strong inner-sphere interactions between CO<sub>2</sub> and the MGE. Herein we report the first successful chemical reduction of CO<sub>2</sub> at room temperature by alkali metals, promoted by a cyclic(alkyl)(amino) carbene (CAAC). One-electron reduction of CAAC-CO<sub>2</sub> adduct (<b>1</b>) with lithium, sodium or potassium metal yields stable monoanionic radicals clusters [M(CAAC–CO<sub>2</sub>)]<sub>n</sub>(M = Li, Na, K, <b> 2</b>-<b>4</b>) and two-electron alkali metal reduction affords open-shell, dianionic clusters of the general formula [M<sub>2</sub>(CAAC–CO<sub>2</sub>)]<sub>n </sub>(<b>5</b>-<b>8</b>). It is notable that these crystalline clusters of reduced CO<sub>2</sub> may also be isolated via the “one-pot” reaction of free CO<sub>2</sub> with free CAAC followed by the addition of alkali metals – a reductive process which does not occur in the absence of carbene. Each of the products <b>2</b>-<b>8</b> were investigated using a combination of experimental and theoretical methods.<br>

A Series of Metal-Organic Frameworks for Selective CO2 Capture and Catalytic Oxidative Carboxylation of Olefins

2018 ◽  
Author(s):  
Huong T. D. Nguyen ◽  
Y B. N. Tran ◽  
Hung N. Nguyen ◽  
Tranh C. Nguyen ◽  
Felipe Gándara ◽  
...  
Keyword(s):  
Room Temperature ◽  
Gas Adsorption ◽  
New Materials ◽  
One Pot ◽  
Acid Gas ◽  
Naphthalene Diimide ◽  
Styrene Carbonate ◽  
Metal Organic ◽  
Adsorption Of Co ◽  
The One

<p>Three novel lanthanide metal˗organic frameworks (Ln-MOFs), namely MOF-590, -591, and -592 were constructed from a naphthalene diimide tetracarboxylic acid. Gas adsorption measurements of MOF-591 and -592 revealed good adsorption of CO<sub>2</sub> (low pressure, at room temperature) and moderate CO<sub>2</sub> selectivity over N<sub>2</sub> and CH<sub>4</sub>. Accordingly, breakthrough measurements were performed on a representative MOF-592, in which the separation of CO<sub>2</sub> from binary mixture containing N<sub>2</sub> and CO<sub>2</sub> was demonstrated without any loss in performance over three consecutive cycles. Moreover, MOF-590, MOF-591, and MOF-592 exhibited catalytic activity in the one-pot synthesis of styrene carbonate from styrene and CO<sub>2</sub> under mild conditions (1 atm CO<sub>2</sub>, 80 °C, and solvent-free). Among the new materials, MOF-590 revealed a remarkable efficiency with exceptional conversion (96%), selectivity (95%), and yield (91%). </p><br>

Flow Chemistry Controls Both Self-Assembly and the Entrapped Oscillatory Cargo in Belousov-Zhabotinsky Driven Polymerization-Induced Self-Assembly

2019 ◽  
Author(s):  
Liman Hou ◽  
Marta Dueñas-Diez ◽  
Rohit Srivastava ◽  
Juan Perez-Mercader
Keyword(s):  
Self Assembly ◽  
Flow Chemistry ◽  
Batch Reactors ◽  
Equilibrium Conditions ◽  
One Pot ◽  
Bz Reaction ◽  
Polymer Vesicles ◽  
Simultaneous Control ◽  
Novel Method ◽  
Continuously Stirred Tank Reactor

<p></p><p>Belousov-Zhabotinsky (B-Z) reaction driven polymerization-induced self-assembly (PISA), or B-Z PISA, is a novel method for the autonomous one-pot synthesis of polymer vesicles from a macroCTA (macro chain transfer agent) and monomer solution (“soup”) containing the above and the BZ reaction components. In it, the polymerization is driven (and controlled) by periodically generated radicals generated in the oscillations of the B-Z reaction. These are inhibitor/activator radicals for the polymerization. Until now B-Z PISA has only been carried out in batch reactors. In this manuscript we present the results of running the system using a continuously stirred tank reactor (CSTR) configuration which offers some interesting advantages.Indeed, by controlling the CSTR parameters we achieve reproducible and simultaneous control of the PISA process and of the properties of the oscillatory cargo encapsulated in the resulting vesicles. Furthermore, the use of flow chemistry enables a more precise morphology control and chemical cargo tuning. Finally, in the context of biomimetic applications a CSTR operation mimics more closely the open non-equilibrium conditions of living systems and their surrounding environments.</p><p></p>

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