Crystallization and structural properties of a family of isotopological 3D-networks: the case of a 4,4′-bipy ligand–M2+ triflate system

CrystEngComm ◽  
2018 ◽  
Vol 20 (26) ◽  
pp. 3784-3795 ◽  
Author(s):  
Silvia Rizzato ◽  
Massimo Moret ◽  
Fabio Beghi ◽  
Leonardo Lo Presti

Desolvation process characterization of a flexible coordination network performed by time-resolved single-crystal X-ray diffraction. Influence of the metal centre on the network stability.

1997 ◽  
Vol 44 (3) ◽  
pp. 950-956 ◽  
Author(s):  
S.L. Barna ◽  
J.A. Shepherd ◽  
M.W. Tate ◽  
R.L. Wixted ◽  
E.F. Eikenberry ◽  
...  

2018 ◽  
Vol 74 (10) ◽  
pp. 1116-1122
Author(s):  
Pheello I. Nkoe ◽  
Hendrik G. Visser ◽  
Chantel Swart ◽  
Alice Brink ◽  
Marietjie Schutte-Smith

The synthesis and characterization of two dinuclear complexes, namelyfac-hexacarbonyl-1κ3C,2κ3C-(pyridine-1κN)[μ-2,2′-sulfanediyldi(ethanethiolato)-1κ2S1,S3:2κ3S1,S2,S3]dirhenium(I), [Re2(C4H8S3)(C5H5N)(CO)6], (1), and tetraethylammoniumfac-tris(μ-2-methoxybenzenethiolato-κ2S:S)bis[tricarbonylrhenium(I)], (C8H20N)[Re2(C7H7OS)3(CO)6], (2), together with two mononuclear complexes, namely (2,2′-bithiophene-5-carboxylic acid-κ2S,S′)bromidotricarbonylrhenium(I), (3), and bromidotricarbonyl(methyl benzo[b]thiophene-2-carboxylate-κ2O,S)rhenium(I), (4), are reported. Crystals of (1) and (2) were characterized by X-ray diffraction. The crystal structure of (1) revealed two Re—S—Re bridges. The thioether S atom only bonds to one of the ReImetal centres, while the geometry of the second ReImetal centre is completed by a pyridine ligand. The structure of (2) is characterized by three S-atom bridges and an Re...Re nonbonding distance of 3.4879 (5) Å, which is shorter than the distance found for (1) [3.7996 (6)/3.7963 (6) Å], but still clearly a nonbonding distance. Complex (1) is stabilized by six intermolecular hydrogen-bond interactions and an O...O interaction, while (2) is stabilized by two intermolecular hydrogen-bond interactions and two O...π interactions.


2009 ◽  
Vol 145 (3-4) ◽  
pp. 188-194 ◽  
Author(s):  
José A. Rodriguez ◽  
Jonathan C. Hanson ◽  
Wen Wen ◽  
Xianqin Wang ◽  
Joaquín L. Brito ◽  
...  

2003 ◽  
Vol 81 (12) ◽  
pp. 1482-1491 ◽  
Author(s):  
Tosha M Barclay ◽  
Ignacio del Río ◽  
Robert A Gossage ◽  
Sarah M Jackson

The synthesis and characterization of 11 zinc halide derivatives that contain monodentate oxazoline ligands is described. The treatment of ether solutions of [ZnX2] (X = Cl, Br, I) with 2-aryl- or 2-methyl-2-oxazolines results in the formation of mildly hygroscopic complexes of the general formulae [ZnX2(ox)2] (ox = 2-methyl-2-oxazoline (1), 2,4,4-trimethyl-2-oxazoline (2), 2-phenyl-2-oxazoline (3), or 4,4-dimethyl-2-phenyl-2-oxazoline (4)), except in the case of ZnI2, which does not form an isolable complex — likely for steric reasons — with oxazoline 4. Treatment of [ZnBr2(4)2] with 1 reveals (1H NMR) that 1 only sluggishly displaces coordinated 4 at temperatures below 50 °C. The structural characterization, via single crystal X-ray diffraction, of six of the complexes, viz. [ZnI2(1)2], [ZnI2(2)2], [ZnX2(3)2] (X = Cl, Br, or I), and [ZnBr2(4)2], is also reported. All of these structurally characterized complexes are mononuclear zinc compounds with an overall distorted tetrahedral arrangement of the two halide and two oxazoline ligands around the zinc metal centre. The oxazoline series of complexes reported herein show little structural diversity, a facet which is in contrast to their substituted pyridine analogues.Key words: oxazoline, zinc, X-ray crystal structure, coordination complex, NMR spectroscopy, Zn(II).


2009 ◽  
Vol 87 (1) ◽  
pp. 368-379 ◽  
Author(s):  
Robert A Gossage ◽  
Paras N Yadav ◽  
Timothy D MacInnis ◽  
J Wilson Quail ◽  
Andreas Decken

The synthesis and characterization of 14 ZnX2 (X = Cl or Br) complexes containing aryl-oxazoline (ox) ligands is reported. Eleven of these derivatives have been structurally elucidated in the solid state by single crystal X-ray diffraction methods. The ligands used are 2-(3-R-phenyl)-2-oxazoline (R = Cl or Me), 2-(4-R-phenyl)-2-oxazoline (R = Cl, F, Me or –OMe), and 2-(anisol-2-yl)-4,4-dimethyl-2-oxazoline (7a). All oxazolines, with the exception of 7a, lead to the formation of materials identified as ZnX2(ox)2 upon reaction with ZnX2. A distorted tetrahedral coordination motif around the Zn metal centre is displayed in nine examples that have been characterized by single crystal X-ray diffraction methods. In the case of ligand 7a, an unusual dimeric species (X-ray) of formula [ZnCl2(7a)]2 (7b) is formed upon reaction with ZnCl2. Compound 7b displays a rare (formally neutral) µ-(Cl)2-(Zn[L]Cl)2 (L = neutral donor ligand) unit in addition to secondary bonding interactions between the Zn centres and the O-atom of the –OMe group (Zn···O distance of ~2.56 Å). In contrast, reactions of 7a with ZnBr2 lead to the formation of a monomeric species containing a chelating molecule of 7a with binding through the oxazoline N-atom and the methoxy (Zn–O distance of ~2.14 Å) group, i.e., ZnBr2(7a-κ2N,OOMe). These complexes are discussed in terms of structurally related Zn species and some comment is made as to the direction to be explored within this series of materials that may lead to further unusual structural diversity.Key words: oxazoline, oxazole, zinc, X-ray crystal structure, coordination complex, Zn(II) halide.


ChemInform ◽  
2009 ◽  
Vol 40 (43) ◽  
Author(s):  
Jose A. Rodriguez ◽  
Jonathan C. Hanson ◽  
Wen Wen ◽  
Xianqin Wang ◽  
Joaquin L. Brito ◽  
...  

2001 ◽  
Vol 74 (5) ◽  
pp. 835-845 ◽  
Author(s):  
Sudip Ray ◽  
Anil K. Bhowmick

Abstract Clay-Polyacrylate hybrid material was prepared from Montmorillonite (M) clay and polytrimethylol propane triacrylate (PA) using intercalation polymerization process. Characterization of the composite was done by x-ray diffraction (XRD), infrared (IR) spectroscopy, scanning electron microscopy (SEM) and energy dispersive x-ray (EDX) techniques. The results show the successful intercalation of PA in the M moiety. The MPA hybrid material was then blended with a polyolefin elastomer, Engage. Tensile and dynamic mechanical properties were measured on the polymer-filler composite and the results showed interaction between the treated clay and the base polymer. There was a significant improvement in modulus, tensile strength and elongation at break of the base polymer as compared to the composite prepared with the untreated clay.


2016 ◽  
Vol 23 (3) ◽  
pp. 700-711 ◽  
Author(s):  
Daniel Schick ◽  
Loïc Le Guyader ◽  
Niko Pontius ◽  
Ilie Radu ◽  
Torsten Kachel ◽  
...  

The slicing facility FemtoSpeX at BESSY II offers unique opportunities to study photo-induced dynamics on femtosecond time scales by means of X-ray magnetic circular dichroism, resonant and non-resonant X-ray diffraction, and X-ray absorption spectroscopy experiments in the soft X-ray regime. Besides femtosecond X-ray pulses, slicing sources inherently also produce a so-called `halo' background with a different time structure, polarization and pointing. Here a detailed experimental characterization of the halo radiation is presented, and a method is demonstrated for its correct and unambiguous removal from femtosecond time-resolved data using a special laser triggering scheme as well as analytical models. Examples are given for time-resolved measurements with corresponding halo correction, and errors of the relevant physical quantities caused by either neglecting or by applying a simplified model to describe this background are estimated.


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