scholarly journals Self-assembly of metallosupramolecular rhombi from chiral concave 9,9’-spirobifluorene-derived bis(pyridine) ligands

2014 ◽  
Vol 10 ◽  
pp. 432-441 ◽  
Author(s):  
Rainer Hovorka ◽  
Sophie Hytteballe ◽  
Torsten Piehler ◽  
Georg Meyer-Eppler ◽  
Filip Topić ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Self Assembly ◽  
The Self ◽  
Assembly Process ◽  
X Ray Diffraction ◽  
X Ray ◽  
Pyridine Ligands ◽  
Racemic Form

Two new 9,9’-spirobifluorene-based bis(4-pyridines) were synthesised in enantiopure and one also in racemic form. These ligands act as concave templates and form metallosupramolecular [(dppp)2M2L2] rhombi with cis-protected [(dppp)Pd]2+ and [(dppp)Pt]2+ ions. The self-assembly process of the racemic ligand preferably occurs in a narcissistic self-recognising manner. Hence, a mixture of all three possible stereoisomers [(dppp)2M2{(R)-L}2](OTf)4, [(dppp)2M2{(S)-L}2](OTf)4, and [(dppp)2M2{(R)-L}{(S)-L}](OTf)4 was obtained in an approximate 1.5:1.5:1 ratio which corresponds to an amplification of the homochiral assemblies by a factor of approximately three as evidenced by NMR spectroscopy and mass spectrometry. The racemic homochiral assemblies could also be characterised by single crystal X-ray diffraction.

Controlled Growth and Self-Assembly of CaCO3 Superstructures between the Organic-Water Interfaces

2010 ◽  
Vol 434-435 ◽  
pp. 597-600
Author(s):  
Xiao Hong Liang ◽  
Jun Hui Xiang ◽  
Fu Shi Zhang ◽  
Li Xing ◽  
Bo Song ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Calcium Carbonate ◽  
Self Assembly ◽  
Crystallization Behavior ◽  
Gas Diffusion ◽  
The Self ◽  
Assembly Process ◽  
X Ray Diffraction ◽  
X Ray ◽  
Scanning Electron

In this paper, the crystallization behavior of calcium carbonate between the organic-water interfaces using a slow gas-diffusion procedure is studied. The organic-water interfaces can control the crystallization of calcium carbonate to form a flower-shaped superstructure. The precipitates of calcium carbonate were identified by X-ray diffraction (XRD) and scanning electron microscopy (SEM). A possible mechanism about the self-assembly process of CaCO3 crystals has been analyzed. It is found that the morphology of CaCO3 superstructure depends on the properties of organic solvent. This paper also presents the influence of surfactant monolayer, between the biphase interfaces, on the CaCO3 superstructure. This study suggests that it is possible to control morphogenesis of calcium carbonate by a combination of a surfactant monolayer with the organic-water interfaces.

Incremental iodination of the eight-vertex closo monocarborane anion [closo-1-CB7H8]–: Preparation and characterization of [closo-1-CB7H5-6,7,8-I3]– and [closo-1-CB7H2-2,3,4,6,7,8-I6]–, and the synthesis of the first eight-vertex C-methylated carborane anion [1-CH3-closo-1-CB7H4-6,7,8-I3]–

2010 ◽  
Vol 75 (9) ◽  
pp. 931-947 ◽  
Author(s):  
Radim Dostál ◽  
Michael G. S. Londesborough ◽  
Magdalena Kvíčalová ◽  
Jan Macháček ◽  
Ivana Císařová ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Electrophilic Substitution ◽  
X Ray Diffraction ◽  
X Ray ◽  
Molecular Behavior ◽  
Elemental Iodine ◽  
Insight Into

Iodination of [closo-1-CB7H8]– (anion 1) with elemental iodine under various controlled conditions yields a continuum from mono- to hexaiodinated derivatives including the previously unknown [closo-1-CB7H5-6,7,8-I3]– (anion 5) and [closo-1-CB7H2-2,3,4,6,7,8-I6]– (anion 8). These species, characterized by mass spectrometry and NMR spectroscopy, and, in the case of 8, by single-crystal X-ray diffraction, provide insight into the fluxional molecular behavior of anion 1 in solution. Investigation of direct electrophilic substitution on the carbon-vertex of anion 1 using standard conditions and reagents (deprotonation by BuLi followed by addition of electrophile) proved futile, but the same conditions when using the new triiodo-deravitive anion 5 resulted in the formation of the first eight-vertex C-methylated carborane anion [1-CH3-closo-1-CB7H4-6,7,8-I3]– (anion 9), in 60% yield.

scholarly journals Order in disorder: solution and solid-state studies of [MIII2MII5] wheels (MIII = Cr, Al; MII = Ni, Zn)

2018 ◽  
Vol 47 (34) ◽  
pp. 11834-11842 ◽  
Author(s):  
Hector W. L. Fraser ◽  
Gary S. Nichol ◽  
Dušan Uhrín ◽  
Ulla Gro Nielsen ◽  
Marco Evangelisti ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Solid State ◽  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Solid State Nmr ◽  
Squid Magnetometry ◽  
X Ray Diffraction ◽  
X Ray ◽  
Solid State Nmr Spectroscopy ◽  
Esi Mass Spectrometry

Heterometallic species with Anderson-like structures are characterised by single-crystal X-ray diffraction, solution- and solid-state NMR spectroscopy, ESI mass spectrometry and SQUID magnetometry.

Dimeres Di(N-lithium–tert–butylamino)bis(dimethylamino)silan - [Si(N(CH3)2)2(NLiC(CH3)3)2]2 – Darstellung und Kristallstruktur / Dimeric Di(N -lithio-tert-butylamino)bis(dimethylamino)silane - [Si(N(CH3)2)2(NLiC(CH3)3)2]2 – Synthesis und Crystal Structure

2001 ◽  
Vol 56 (1) ◽  
pp. 90-94 ◽  
Author(s):  
Josef Engering ◽  
Eva-Maria Peters ◽  
Martin Jansen
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Solid State ◽  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Title Compound ◽  
Solution Nmr ◽  
X Ray Diffraction ◽  
X Ray ◽  
Solution Nmr Spectroscopy

Abstract [Si(N(CH3)2)2(NLiC(CH3)3)2]2 results from the reaction of silicon tetrachloride with excess terf-butylamine, followed by halogen substitution with LiN(CH3)2, and treatment with n-butyllithium in hexane. The title compound, found to be dimeric in the solid state, was characterised by single crystal X-ray diffraction (triclinic, Pi , a = 10.208(2), b = 12.140(2), c = 15.658(3) Å , a = 79.02(3), ß = 82.80(3), γ = 67.19(3)°, Z = 2, C24H60Li4N8Si2 ), and by solid state and solution NMR-spectroscopy and mass spectrometry.

Formation of a [2]rotaxane and [2]catenane based on PdBr2L2 as a template

2009 ◽  
Vol 87 (1) ◽  
pp. 205-211 ◽  
Author(s):  
Barry A Blight ◽  
James A Wisner ◽  
Michael C Jennings
Keyword(s):  
Hydrogen Bond ◽  
Hydrogen Bonding ◽  
Nmr Spectroscopy ◽  
Supramolecular Chemistry ◽  
Self Assembly ◽  
The Self ◽  
X Ray Diffraction ◽  
Template Effect ◽  
X Ray ◽  
The Poor

Previous studies have determined that neutral palladium(II) dibromide complexes template the formation of [2]pseudorotaxanes, albeit with weaker affinities than the analogous palladium(II) dichloride species. Here, the self-assembly of both [2]rotaxane (2) and [2]catenane (5) were attempted using a PdBr2L2 centre as the template, resulting in the desired interlocked structures. The structures were confirmed by NMR spectroscopy, CSI-MS, and single crystal X-ray diffraction analyses. [2]Rotaxane 2 was isolated in 53% and [2]catenane 5 in 41% yields. The lower yields observed in comparison to the chloride analogues can be attributed to the reduced template effect of the palladium(II) dibromide subunits, caused by both the poor steric fit of the bromides in the isophthalamide cleft and bromide’s reduced capacity as a hydrogen bond acceptor.Key words: rotaxane, catenane, hydrogen bonding, interlocked, supramolecular chemistry.

scholarly journals Pourous nanoparticles formation using a dendrimer template

2010 ◽  
Vol 24 (3-4) ◽  
pp. 427-431
Author(s):  
L. Bonaccorsi ◽  
D. Lombardo ◽  
A. Longo ◽  
E. Proverbio ◽  
P. Calandra
Keyword(s):  
Self Assembly ◽  
Particle Interaction ◽  
Pamam Dendrimer ◽  
The Self ◽  
Assembly Process ◽  
X Ray Diffraction ◽  
X Ray ◽  
X Ray Scattering ◽  
Zeolite Lta ◽  
Scanning Electron

We describe the synthesis of porous spherical nanoaggregates derived by the controlled growth of zeolite LTA on a poliamidoamine (Pamam) dendrimer acting as nano-template. The presence of a strong condensed cationic Na+charge all around the dendrimers, which is responsible for the intense electrostatic inter-particle interaction potential, stimulate the condensed growth of the zeolitic phase onto the dendrimer substrate. Moreover, the screening produced by the zeolite grown on the dendrimer surface promote the entanglement process between the primary units with the formation of large porous clusters. The main features of the self-assembly process has been characterised by means of different techniques such as Small Angle X-ray Scattering (SAXS), Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD) and Energy Dispersive X-ray (EDX) microprobe spectroscopy. The finding of our results may open new perspectives in the synthesis of organic–inorganic nanostructured materials based on mesoporous frameworks with new characteristics and properties.

Unraveling the Self-Assembly Modes in Multicomponent Supramolecular Gels Using Single-Crystal X-ray Diffraction

2020 ◽  
Vol 32 (8) ◽  
pp. 3517-3527 ◽  
Author(s):  
Dipankar Ghosh ◽  
Abbas D. Farahani ◽  
Adam D. Martin ◽  
Pall Thordarson ◽  
Krishna K. Damodaran
Keyword(s):  
Single Crystal ◽  
Self Assembly ◽  
The Self ◽  
X Ray Diffraction ◽  
X Ray ◽  
Supramolecular Gels

N-Dimethylphosphinoyl-substituted Aminomethanephosphonic Acids

2010 ◽  
Vol 65 (5) ◽  
pp. 556-564 ◽  
Author(s):  
Victoria Lachkova ◽  
Sabi Varbanov ◽  
Walter Frank ◽  
Helmut Keck
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Electrospray Ionization ◽  
Elemental Analysis ◽  
Electrospray Ionization Mass Spectrometry ◽  
Ionization Mass ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr

Three new N-phosphinoyl-substituted aminomethanephosphonic acids have been synthesized and characterized: dimethylphosphinoylmethyl-imino-bis(methanephosphonic acid) (1), [3-(dimethylphosphinoyl)-propyl]-imino-bis(methanephosphonic acid) (2), and N-benzyl-Ndimethylphosphinoylmethyl- aminomethanephosphonic acid (3). The latter was isolated as a hydrochloride 3 ・ HCl. The acids have been prepared via Moedritzer-Irani reaction from the corresponding dimethylphosphinoyl-substituted primary and secondary aliphatic amines. Their structures have been confirmed by elemental analysis, IR, 1H, 31P{1H}, 13C{1H} NMR spectroscopy, electrospray ionization mass spectrometry, and single-crystal X-ray diffraction.

Synthesis and Characterization of 3-Chloropropyl-substituted o- Carboranes: Crystal Structures of 1,2-(1,3-Propanediyl)-o-carborane, 1-(3-Chloropropyl)-o-carborane and 1,2-Bis(3-chloropropyl)-ocarborane

2013 ◽  
Vol 68 (7) ◽  
pp. 804-810 ◽  
Author(s):  
Deqian Bian ◽  
Yong Nie ◽  
Jinling Miao ◽  
Zhenwei Zhang ◽  
Ping Lu
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Main Product ◽  
Total Yield ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ir And Nmr Spectroscopy

The reactions of the lithio-o-carborane Li2C2B10H10 with ClCH2CH2CH2Br were studied under various conditions. While the main product is the known exo-polyhedrally cyclized 1,2- (1,3-propanediyl)-o-carborane (2), the expected 3-chloropropyl-substituted carborane products 1- (ClCH2CH2CH2)C2B10H11 (3) and 1,2-(ClCH2CH2CH2)2C2B10H10 (4) can be obtained in a total yield of 22%. In the presence of CuCl, the same reaction proceeded rather slowly and gave compound 3and bis(o-carborane) (5) in small yields, with the recovery of the starting o-C2B10H12. Compounds 2- 4were characterized by means of IR and NMR spectroscopy and mass spectrometry, as well as by single-crystal X-ray diffraction.

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