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 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.

scholarly journals Exploring the Structural Chemistry of Pyrophosphoramides: N,N′,N″,N‴-Tetraisopropylpyrophosphoramide

Chemistry ◽  
2021 ◽  
Vol 3 (1) ◽  
pp. 149-163
Author(s):  
Duncan Micallef ◽  
Liana Vella-Zarb ◽  
Ulrich Baisch
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nuclear Magnetic Resonance ◽  
Hydrogen Bonding ◽  
Nmr Spectroscopy ◽  
Ir Spectroscopy ◽  
Room Temperature ◽  
Intermolecular Hydrogen Bonding ◽  
X Ray Diffraction ◽  
X Ray

N,N′,N″,N‴-Tetraisopropylpyrophosphoramide 1 is a pyrophosphoramide with documented butyrylcholinesterase inhibition, a property shared with the more widely studied octamethylphosphoramide (Schradan). Unlike Schradan, 1 is a solid at room temperature making it one of a few known pyrophosphoramide solids. The crystal structure of 1 was determined by single-crystal X-ray diffraction and compared with that of other previously described solid pyrophosphoramides. The pyrophosphoramide discussed in this study was synthesised by reacting iso-propyl amine with pyrophosphoryl tetrachloride under anhydrous conditions. A unique supramolecular motif was observed when compared with previously published pyrophosphoramide structures having two different intermolecular hydrogen bonding synthons. Furthermore, the potential of a wider variety of supramolecular structures in which similar pyrophosphoramides can crystallise was recognised. Proton (1H) and Phosphorus 31 (31P) Nuclear Magnetic Resonance (NMR) spectroscopy, infrared (IR) spectroscopy, mass spectrometry (MS) were carried out to complete the analysis of the compound.

The Evaluation of TiTe2 as a Diffusion Barrier in the Formation of Low Thermal Conductivity Nanolaminates with Bi2Te3 and Sb2Te3

2010 ◽  
Vol 74 ◽  
pp. 38-47
Author(s):  
Clay Mortensen ◽  
Paul Zschack ◽  
David C. Johnson
Keyword(s):  
Thermal Conductivity ◽  
Diffusion Barrier ◽  
Self Assembly ◽  
Low Temperatures ◽  
Annealing Temperature ◽  
The Self ◽  
High Angle ◽  
X Ray Diffraction ◽  
Amorphous Precursor ◽  
X Ray

The evolution of designed [(Ti-Te)]x[(Sb-Te)]y, [(Bi-Te)]x[(Sb-Te)]y, [(Ti-Te)]w[(Bi-Te)]x[(Sb-Te)]y and [(Ti-Te)]w[(Bi-Te)]x[(Ti-Te)]y[(Sb-Te)]z precursors were followed as a function of annealing temperature and time using both low and high angle x-ray diffraction techniques to probe the self assembly into nanolaminate materials. The [(Bi-Te)]x[(Sb-Te)]y precursors were found to interdiffuse at low temperatures to form a (BixSb1-x)2Te3 alloy. The [(Ti-Te)]x[(Bi-Te)]y and [(Ti-Te)]x[(Sb-Te)]y precursors formed ordered nanolaminates [{(TiTe2)}1.35]x[Bi2Te3]y and [{(TiTe2)}1.35]x[Sb2Te3]y respectively. The [(Ti-Te)]w[(Bi-Te)]x[(Sb-Te)]x precursors formed [{(TiTe2)}1.35]w[(Bi0.5Sb0.5)2Te3]2x nanolaminates on annealing, as the bismuth and antimony layers interdiffused. Over the range of TiTe2 thicknesses used in [(Ti-Te)]w[(Bi-Te)]x[(Ti-Te)]y[(Sb-Te)]z precursors, Bi and Sb were found to interdiffuse through the 2-4 nm thick Ti-Te layers, resulting in the formation of (BixSb1-x)2Te3 alloy layers as part of the final nanolaminated products. When the Bi-Te and Sb-Te thicknesses were equal in the amorphous precursors, symmetric [{(TiTe2)}1.35]m[(Bi0.5Sb0.5)2Te3]n nanolamiantes were formed. When the thicknesses of Bi-Te and Sb-Te layers were not equal in the amorphous precursor, asymmetric [(TiTe2)1.35]m[(BixSb1-x)2Te3]n[(TiTe2)1.35]m[(BixSb1-x)2Te3]p nanolaminates were formed. These results imply that to form (A)w(B)x(C)y nanolaminates using designed layered precursors all three components must be immiscible. To form (A)x(B)y(A)x(C)z nanolaminates, the components must be immiscible or the precursor to the A component and the A component itself must be an effective interdiffusion barrier preventing B and C from mixing.

Hydrothermal Syntheses, Crystal Structures, and Luminescent Properties of Two MnII Coordination Polymers: From Two-Fold Interpenetrated pcu Topological Net to Polycatenated 2D+2D→3D Framework

2015 ◽  
Vol 68 (2) ◽  
pp. 322 ◽  
Author(s):  
Wenlong Liu ◽  
Mengqiang Wu ◽  
Xueying Wang ◽  
Wei Wang ◽  
Dayu Liu ◽  
...  
Keyword(s):  
Dicarboxylic Acid ◽  
Coordination Polymers ◽  
Self Assembly ◽  
Room Temperature ◽  
Luminescent Properties ◽  
The Self ◽  
X Ray Diffraction ◽  
X Ray ◽  
3D Framework ◽  
Dimethyl Benzene

Using a hydrothermal synthesis, the self-assembly of MnII ions and 1,4-bis(1-imidazol-yl)-2,5-dimethyl benzene with two dicarboxylate ligands, 2-nitrobenzene-1,4-dicarboxylic acid (2-H2ata) and 5-methylbenzene-1,3-dicarboxylic acid (5-CH3-H2ip) constructed two interesting coordination polymers: [Mn(2-ata)(bimb)]n (1) and {[Mn(5-CH3-ip)(bimb)1.5]·2H2O}n (2), where bimb refers to 1,4-bis(1-imidazol-yl)-2,5-dimethyl benzene. Their structures were determined by single-crystal X-ray diffraction, elemental analysis, and infrared spectroscopy. Complex 1 exhibits a 2-fold interpenetrated pcu net. Complex 2 shows an unusual polycatenated 2D+2D→3D framework. In addition, the solid-state photoluminescent properties of 1 and 2 were investigated at room temperature.

Construction of a three-dimensional supramolecular framework based on an anionic cadmium(II) coordination network and protonated dipyridine organic cations

2018 ◽  
Vol 74 (8) ◽  
pp. 889-893
Author(s):  
Qian-Kun Zhou ◽  
Lin Wang ◽  
Dong Liu
Keyword(s):  
Hydrogen Bonding ◽  
Self Assembly ◽  
Title Compound ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
Hydrothermal Conditions ◽  
X Ray ◽  
Coordination Network ◽  
Hydrogen Bonding Interactions ◽  
Point Symbol

As a class of multifunctional materials, crystalline supramolecular complexes have attracted much attention because of their unique architectures, intriguing topologies and potential applications. In this article, a new supramolecular compound, namely catena-poly[4,4′-(buta-1,3-diene-1,4-diyl)dipyridin-1-ium [(μ4-benzene-1,2,4,5-tetracarboxylato-κ6 O 1,O 1′:O 2:O 4,O 4′:O 5)cadmium(II)]], {(C14H14N2)[Cd(C10H2O8)]} n or {(1,4-H2bpbd)[Cd(1,2,4,5-btc)]} n , has been prepared by the self-assembly of Cd(NO3)2·4H2O, benzene-1,2,4,5-tetracarboxylic acid (1,2,4,5-H4btc) and 1,4-bis(pyridin-4-yl)buta-1,3-diene (1,4-bpbd) under hydrothermal conditions. The title compound has been structurally characterized by IR spectroscopy, elemental analysis, powder X-ray diffraction and single-crystal X-ray diffraction analysis. Each CdII centre is coordinated by six O atoms from four different (1,2,4,5-btc)4− tetraanions. Each CdII cation, located on a site of twofold symmetry, binds to four carboxylate groups belonging to four separate (1,2,4,5-btc)4− ligands. Each (1,2,4,5-btc)4− anion, situated on a position of \overline{1} symmetry, binds to four crystallographically equivalent CdII centres. Neighbouring CdII cations interconnect bridging (1,2,4,5-btc)4− anions to form a three-dimensional {[Cd(1,2,4,5-btc)]2−} n anionic coordination network with infinite tubular channels. The channels are visible in both the [1\overline{1}0] and the [001] direction. Such a coordination network can be simplified as a (4,4)-connected framework with the point symbol (4284)(4284). To balance the negative charge of the metal–carboxylate coordination network, the cavities of the network are occupied by protonated (1,4-H2bpbd)2+ cations that are located on sites of twofold symmetry. In the crystal, there are strong hydrogen-bonding interactions between the anionic coordination network and the (1,4-H2bpbd)2+ cations. Considering the hydrogen-bonding interactions, the structure can be further regarded as a three-dimensional (4,6)-connected supramolecular architecture with the point symbol (4264)(42687·84). The thermal stability and photoluminescence properties of the title compound have been investigated.

Molecular Cocrystals of Carboxylic Acids. XXVI Adducts of the Amino-Substituted Benzoic Acids with Nitroaromatic Lewis Bases: the Influence of Associative Polyfunctional Substituents on Self-Assembly of Molecules in Cocrystallization Processes

1997 ◽  
Vol 50 (10) ◽  
pp. 977 ◽  
Author(s):  
Daniel E. Lynch ◽  
Graham Smith ◽  
Karl A. Byriel ◽  
Colin H. L. Kennard
Keyword(s):  
Hydrogen Bonding ◽  
Infrared Spectroscopy ◽  
Self Assembly ◽  
Benzoic Acids ◽  
Aminobenzoic Acid ◽  
X Ray Diffraction ◽  
X Ray ◽  
Lewis Bases ◽  
Aminobenzoic Acids ◽  
Substituted Benzoic Acids

A series of molecular adducts of the isomeric aminobenzoic acids with the nitro-substituted Lewis bases 2-chloro-5-nitropyridine, 5-nitroquinoline and 5-nitroisoquinoline has been prepared and characterized by using infrared spectroscopy and X-ray powder diffraction, and in four cases by single-crystal X-ray diffraction methods. These four compounds are the adducts of 3-aminobenzoic acid with 5-nitroquinoline [(C7H7NO2)(C9H6N2O2)], 4-aminobenzoic acid with 5-nitroquinoline [(C7H7NO2)2(C9H6N2O2)], 2-aminobenzoic acid with 5-nitroisoquinoline [(C7H7NO2)(C9H6N2O2)] and 4-aminobenzoic acid with 5-nitroisoquinoline [(C7H7N2O2)(C9H6N2O2)]. Other compounds described are the (1 : 1) adducts of 4-aminobenzoic acid with 2-chloro-5-nitropyridine, and 2-aminobenzoic acid with 5-nitroquinoline. All adducts involve hydrogen-bonding network associations while in none of the examples is any proton transfer involved.

Synthese und Koordinationschemie eines neuartigen Bistetrazols: Ein 1D-Metallopolymer durch Selbstorganisation koordinativ ungesättigter Zink(II)-M4onomere [1] / Synthesis and Coordination Chemistry of a New Bistetrazole: A 1D-Metallopolymer via Self-Assembly of Monomeric Zinc(II)-Buildingblocks

1995 ◽  
Vol 50 (4) ◽  
pp. 642-648 ◽  
Author(s):  
Rolf W. Saalfrank ◽  
Klaus Schobert ◽  
Stefan Trümmer ◽  
Alexander Wolski
Keyword(s):  
Coordination Chemistry ◽  
Self Assembly ◽  
Intermediate Formation ◽  
The Self ◽  
Polymeric Chain ◽  
X Ray Diffraction ◽  
Bridging Ligands ◽  
Subsequent Formation ◽  
X Ray ◽  
Polymeric Compounds

The new bistetrazole 13 has been obtained by subsequent formation of the two heterocyclic units. In methanolic solution 13 reacts with zinc(II) acetate to yield the pseudo-meso-1 D-coordination polymer [ZnL2(MeOH)]n (n = ∞) 14. The structure of 14 was established by single crystal X-ray diffraction. The generation of the polymeric chain 14 is understandable, if intermediate formation of coordinatively unsaturated zinc(II) buildingblocks (Δ)-15 and (Λ)-15 is assumed. Alternating linkage of the self-complementary chiral monomers 15, across one cyanofunction each, leads to 14 with zinc being essentially octahedrally coordinated. Compared with polymeric compounds of similar bridging ligands, the Zn ··· N≡C-distance in 14 (225,7 pm) is short.

Fabrication and Hydrogen Sensing Property of In2O3 Nanotowers

2013 ◽  
Vol 834-836 ◽  
pp. 913-916
Author(s):  
Zhao Qiang Zheng ◽  
Huan Yu Wu ◽  
Bing Wang
Keyword(s):  
Self Assembly ◽  
Thermal Evaporation ◽  
Sensor Response ◽  
The Self ◽  
X Ray Diffraction ◽  
Excellent Performance ◽  
X Ray ◽  
Hydrogen Sensing ◽  
Morphology And Structure ◽  
Prepared Nanorods

In2O3nanotowers have been fabricated on Au item-shaped parallel electrodes using thermal evaporation of the mixed powders of In2O3and graphite with Au catalysts. The morphology and structure of the prepared nanorods are determined on the basis of field-emission scanning electron microscopy (FESEM) and x-ray diffraction (XRD). The self-assembly grown sensors of In2O3nanotowers have excellent performance in sensor response to hydrogen concentration of 1000 ppm under operated temperature of 300°C.

Two new isostructural mercury(II) complexes involving the N-heterocyclic 1-[(benzotriazol-1-yl)methyl]-1H-1,3-imidazole ligand: syntheses, structures and properties

2017 ◽  
Vol 73 (4) ◽  
pp. 314-318 ◽  
Author(s):  
Xu Wei ◽  
Jian-Hua Li ◽  
Qiu-Ying Huang ◽  
Xiang-Ru Meng
Keyword(s):  
Solid State ◽  
Hydrogen Bonds ◽  
Ir Spectra ◽  
Self Assembly ◽  
Three Dimensional ◽  
The Self ◽  
X Ray Diffraction ◽  
X Ray ◽  
Heterocyclic Ligand ◽  
Structures And Properties

The unsymmetrical N-heterocyclic ligand 1-[(benzotriazol-1-yl)methyl]-1H-1,3-imidazole (bmi) has three potential N-atom donors and can act in monodentate or bridging coordination modes in the construction of complexes. In addition, the bmi ligand can adopt different coordination conformations, resulting in complexes with different structures due to the presence of the flexible methylene spacer. Two new complexes, namely bis{1-[(benzotriazol-1-yl)methyl]-1H-1,3-imidazole-κN3}dibromidomercury(II), [HgBr2(C10H9N5)2], and bis{1-[(benzotriazol-1-yl)methyl]-1H-1,3-imidazole-κN3}diiodidomercury(II), [HgI2(C10H9N5)2], have been synthesized through the self-assembly of bmi with HgBr2or HgI2. Single-crystal X-ray diffraction shows that both complexes are mononuclear structures, in which the bmi ligands coordinate to the HgIIions in monodentate modes. In the solid state, both complexes display three-dimensional networks formed by a combination of hydrogen bonds and π–π interactions. The IR spectra and PXRD patterns of both complexes have also been recorded.

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