Creation and stabilisation of tuneable open metal sites in thiocyanato-bridged heterometallic coordination polymers to be used as heterogeneous catalysts

2019 ◽  
Vol 48 (45) ◽  
pp. 17063-17069 ◽  
Author(s):  
Hiroyasu Tabe ◽  
Masaaki Matsushima ◽  
Rika Tanaka ◽  
Yusuke Yamada
Keyword(s):  
Single Crystal ◽  
Coordination Polymers ◽  
Heterogeneous Catalysts ◽  
X Ray ◽  
Open Metal Sites ◽  
Heterometallic Coordination Polymers

A series of {MII[PtIV(SCN)6]}n and {MII(CH3OH)x[PtIV(SCN)6]}n were characterised by single-crystal X-ray analyses and examined as heterogeneous catalysts to clarify the requisites for better catalysis.

scholarly journals Pyrene Carboxylate Ligand Based Coordination Polymers for Microwave-Assisted Solvent-Free Cyanosilylation of Aldehydes

Molecules ◽  
2021 ◽  
Vol 26 (4) ◽  
pp. 1101
Author(s):  
Anirban Karmakar ◽  
Anup Paul ◽  
Elia Pantanetti Sabatini ◽  
M. Fátima C. Guedes da Silva ◽  
Armando J. L. Pombeiro
Keyword(s):  
Coordination Polymer ◽  
Single Crystal ◽  
Coordination Polymers ◽  
Metal Ion ◽  
Solvent Free ◽  
Lewis Acidity ◽  
Carboxylate Ligand ◽  
X Ray Diffraction ◽  
X Ray ◽  
Microwave Assisted

The new coordination polymers (CPs) [Zn(μ-1κO1:1κO2-L)(H2O)2]n·n(H2O) (1) and [Cd(μ4-1κO1O2:2κN:3,4κO3-L)(H2O)]n·n(H2O) (2) are reported, being prepared by the solvothermal reactions of 5-{(pyren-4-ylmethyl)amino}isophthalic acid (H2L) with Zn(NO3)2.6H2O or Cd(NO3)2.4H2O, respectively. They were synthesized in a basic ethanolic medium or a DMF:H2O mixture, respectively. These compounds were characterized by single-crystal X-ray diffraction, FTIR spectroscopy, thermogravimetric and elemental analysis. The single-crystal X-ray diffraction analysis revealed that compound 1 is a one dimensional linear coordination polymer, whereas 2 presents a two dimensional network. In both compounds, the coordinating ligand (L2−) is twisted due to the rotation of the pyrene ring around the CH2-NH bond. In compound 1, the Zn(II) metal ion has a tetrahedral geometry, whereas, in 2, the dinuclear [Cd2(COO)2] moiety acts as a secondary building unit and the Cd(II) ion possesses a distorted octahedral geometry. Recently, several CPs have been explored for the cyanosilylation reaction under conventional conditions, but microwave-assisted cyanosilylation of aldehydes catalyzed by CPs has not yet been well studied. Thus, we have tested the solvent-free microwave-assisted cyanosilylation reactions of different aldehydes, with trimethylsilyl cyanide, using our synthesized compounds, which behave as highly active heterogeneous catalysts. The coordination polymer 1 is more effective than 2, conceivably due to the higher Lewis acidity of the Zn(II) than the Cd(II) center and to a higher accessibility of the metal centers in the former framework. We have also checked the heterogeneity and recyclability of these coordination polymers, showing that they remain active at least after four recyclings.

Konkurrierende Liganden: Theophyllin als nicht- und stark koordinierender Ligand in Quecksilber(II)-Komplexen / Competing Ligands: Theophylline as Non- and Strongly Coordinating Ligand in Mercury(II) Complexes

2006 ◽  
Vol 61 (6) ◽  
pp. 758-765 ◽  
Author(s):  
Matthias Nolte ◽  
Ingo Pantenburg ◽  
Gerd Meyer
Keyword(s):  
Oxygen Atom ◽  
Water Molecule ◽  
Aqueous Solutions ◽  
Single Crystal ◽  
Coordination Polymers ◽  
Water Molecules ◽  
Slow Evaporation ◽  
Monoclinic Symmetry ◽  
X Ray ◽  
Chloride Ligand

[{Hg(CF3)2}(ThpH)(H2O)](H2O) (1), [{Hg4(Thp)4}(ClO4)4(H2O)8](H2O)4 (2), [{Hg(ThpH)2} (NO3)](NO3) (3) and {Hg(Thp)Cl}(H2O) (4) (ThpH = theophylline, C7H8N4O2) have been synthesized by slow evaporation of aqueous solutions of the mercuric salts Hg(CF3)2, Hg(ClO4)2, Hg(NO3)2, or HgCl2 and theophylline. Their crystal structures were determined on the basis of single crystal X-ray data. The coordination polymers 1 and 2 crystallize with triclinic symmetry, P1̅ (no. 2), with a = 468.8(2), b = 1256.4(5), c = 1445.5(6) pm, α = 67.15(3), β = 89.21(3), γ = 89.40(3)° and a = 833.6(1), b = 1862.7(2), c = 2182.9(2) pm, α = 111.61(1), β = 90.98(1), γ = 95.51(1)°, respectively. 3 and 4 crystallize with monoclinic symmetry, Pc (no. 7), a =1194.1(1), b=1258.8(2), c=735.5(2) pm, β =96.96(2)° and P21/n (no. 14), a=1069.0(2), b =911.6(1), c=1089.9(2) pm and β = 96.87(2)°. In 1 the theophylline molecules are non-coordinating to mercury and leave the Hg(CF3)2 molecule unchanged. Only weak electrostatic attractions to one keto-oxygen atom of theophylline and one water molecule hold this co-crystallisate together. In 2, the theophyllinate anion, Thp−, strongly coordinates with both N(7) and N(9) to HgII forming a large ring with eight Hg atoms that incorporates the water molecules. One sort of nitrate ions in 3 is weakly attached to HgII with the theophylline molecules still bound strongly through N(9). The chloride ligand and the theophyllinate ion seem to have the same strengths as ligands in 4 as they are both attached to HgII with the shortest distances possible

scholarly journals Structural Diversity of Six Coordination Polymers Based on the Designed X-Shaped Ligand 1,1,1,1-Tetrakis[(3-pyridiniourea)methyl]methane

Molecules ◽  
2018 ◽  
Vol 23 (9) ◽  
pp. 2292 ◽  
Author(s):  
Qi-Long Zhang ◽  
Qing Yu ◽  
Hai-Fang Xie ◽  
Bo Tu ◽  
Hong Xu ◽  
...  
Keyword(s):  
Metal Ions ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
Coordination Polymers ◽  
Chain Complex ◽  
Structural Diversity ◽  
Structural Comparison ◽  
Single Crystal Diffraction ◽  
X Ray ◽  
Loop Chain

In this study, six coordination polymers (CPs), {[Ag2(L)(CF3SO3)]·CF3SO3·2H2O·DMF}n (1), {[Ag(L)]·SbF6·4DMF·H2O}n (2), {[Zn(L)0.5(I)2]·3.75H2O}n (3), {[Cd2(L)(I)4(H2O)(DMF)]·4H2O·3DMF}n (4), {[Hg2(L)(I)4]·H2O·4DMF}n (5) and {[Hg2(L)(Cl)4]·2H2O·3DMF}n (6), were obtained based on the designed X-shaped urea-based ligand. X-ray single crystal diffraction analysis revealed that complex 1 displayed a 3D (3,4)-connected {6·82}{64·82}-tcj net. Complex 2 featured a 2D 4-connected {43·63} sheet. Complexes 3 and 5 exhibited a 1D polymeric loop chain. Complex 4 displayed a 1D polymeric fishbone chain. Complex 6 showed a 2D 4-connected {44·62}-sql sheet. Structural comparison revealed that not only the metal ions, but also the anions played crucial roles in the control of final structures.

Assembly of Three Lanthanide Coordination Polymers from 2-(4-Carboxybenzyloxy) Benzoic Acid Ligand: Synthesis, Structure, and Fluorescent Properties

2020 ◽  
Vol 73 (1) ◽  
pp. 16
Author(s):  
Shu-Ju Wang ◽  
Yi-Hui Jiang ◽  
Han-Lin Wu ◽  
Li-Xin You ◽  
Gang Xiong ◽  
...  
Keyword(s):  
Benzoic Acid ◽  
Single Crystal ◽  
Coordination Polymers ◽  
Lanthanide Ions ◽  
Solvothermal Reaction ◽  
X Ray Diffraction ◽  
Fluorescent Properties ◽  
Single Crystal Diffraction ◽  
X Ray ◽  
1D Chain

Three new coordination polymers, {[Ln(cbb)(Hcbb)(DMF)·H2O]n, Ln=Sm (1), Eu (2), Tb(3), H2cbb=2-(4-carboxybenzyloxy) benzoic acid, DMF=N,N-dimethylformamide}, have been synthesised by a solvothermal reaction and structurally characterised by infrared spectroscopy, elemental analysis, thermogravimetry analysis, and X-ray single-crystal diffraction. The results of single-crystal X-ray diffraction indicate that the coordination polymers 1–3 are isostructural, belong to a triclinic system, space group P-1, and show 1D chain structures through the H2cbb ligands connecting adjacent lanthanide ions. In addition, the fluorescence properties of polymers 1–3 were also investigated.

The Syntheses and Structures of Two New Zn(II) Complexes Based on 3-Nitrobenzoato Ligand

2013 ◽  
Vol 807-809 ◽  
pp. 2671-2674
Author(s):  
Ying Bing Lu ◽  
Fang Mei Jian ◽  
Shuang Jin
Keyword(s):  
Single Crystal ◽  
Coordination Polymers ◽  
Stacking Interactions ◽  
X Ray Diffraction ◽  
X Ray ◽  
Face To Face ◽  
Π Interactions ◽  
Carboxylate Groups ◽  
Supramolecular Chain ◽  
Supramolecular Layer

Two new Zn (II) coordination polymers with 3-nitrobenzoato ligands have been prepared, and their structures have been characterized by single-crystal X-ray diffraction techniques. The structure of [Zn (3-nbz)2(μ-4,4'-bpy)]n(1) (3-nbz = 3-nitrobenzoato, 4,4'-bpy = 4,4'-bipyridine) shows 1-D chains originating from terminal 3-nbz ligands andμ-4,4'-bpy molecules. The chains are further connected through face-to-face π stacking interactions to genenate a 2-D supramolecular layer. In Zn (3-nbz)2(2,2'-bpy) (2) (2,2'-bpy = 2,2'-bipyridine), carboxylate groups exhibit chelated bidentate to give discrete mononuclear units, which are linked by face-to-face π-π and C-H···π interactions to produce a 1-D supramolecular chain.

Eindimensionale Kupfer(II)-Koordinationspolymere: Kristall-Engineering durch variable Verknüpfungsmuster [1] / One Dimensional Copper(II) Coordination Polymers: Crystal Engineering through Variable Types of Linkage [1]

1997 ◽  
Vol 52 (1) ◽  
pp. 125-134 ◽  
Author(s):  
Rolf W. Saalfrank ◽  
Roland Harbig ◽  
Oliver Struck ◽  
Frank Hampel ◽  
Eva Maria Peters ◽  
...  
Keyword(s):  
Coordination Polymer ◽  
Single Crystal ◽  
Coordination Polymers ◽  
Crystal Engineering ◽  
Coordination Compounds ◽  
Acetate Solution ◽  
X Ray Diffraction ◽  
One Dimensional ◽  
X Ray ◽  
1D Coordination Polymer

Reaction of a methanolic copper(II) acetate solution with tetrazolyl enol derivatives 2a or 2b leads to the formation of the corresponding lD-coordination polymer 1∞[CuL2] 3a and pseudo 1D-coordination polymer [CuL2]2 3b, respectively. On the contrary, reaction of 2c with methanolic copper(II) acetate solution yields OH-bridged 1D-coordination polymer 1∞[CuL2(MeOH)2 3c. Single-crystal X-ray diffraction of the supramolecular species 3 established unequivocally the structures of the stairlike coordination compounds. Reaction of a methanolic copper(II) acetate solution with amidotetrazole derivative 6 leads to the formation of the lD-coordination polymer 1∞ [CuL2] 7. The structure of 7 has been established by X-ray structure analysis

A Series of Enthalpy/Entropy-Driven Reversible Dissolution/Reorganization Equilibriums in the System of Cu(NO3)2–HL–GdX3–H2O (HL=5-methylpyrazine-2-carboxylic acid; X=Cl, Br, NO3, ClO4)

2014 ◽  
Vol 67 (11) ◽  
pp. 1679
Author(s):  
Sheng Zhang ◽  
Qi Yang ◽  
Xiangyu Liu ◽  
Gang Xie ◽  
Qing Wei ◽  
...  
Keyword(s):  
Thermal Stability ◽  
Magnetic Property ◽  
Structural Analysis ◽  
Carboxylic Acid ◽  
Single Crystal ◽  
Coordination Polymers ◽  
X Ray Diffraction ◽  
X Ray ◽  
2D Network ◽  
Thermal Stability Of

Five coordination polymers, [Cu(L)2]n (1), {[Cu(L)(Cl)(H2O)]·H2O}2n (2), [KCu(L)(μ-Cl)2]n (3), [Cu(L)(Br)H2O]n (4), and {[Cu0.5(HL)(H2O)](NO3)·H2O}2n (5) (HL = 5-methylpyrazine-2-carboxylic acid) were obtained by reactions of a pyramidal CuII-containing ligand, {[Cu(L)2(H2O)]·3H2O}n (LCu), with Gd(ClO4)3·6H2O, GdCl3·6H2O, GdCl3·6H2O/KCl, GdBr3·6H2O, or Gd(NO3)3·6H2O in water. Structural analysis reveals that the structures of these compounds range from a 0D block to a 2D network with modification of the environment of the CuII ions compared with LCu. Interestingly, there occurred a series of reversible dissolution/reorganization equilibriums between the initial reactants and the final products 1–5, which were determined as enthalpy/entropy driven chemical equilibriums by single crystal X-ray diffraction and microcalorimetry. In addition, the thermal stability of 1–4 and the magnetic property of 2 are discussed.

scholarly journals Coordination Polymers of Scandium(III) and Thiophenedicarboxylic Acid

2021 ◽  
Vol 47 (9) ◽  
pp. 593-600
Author(s):  
A. A. Lysova ◽  
V. A. Dubskikh ◽  
K. D. Abasheeva ◽  
A. A. Vasileva ◽  
D. G. Samsonenko ◽  
...  
Keyword(s):  
Ir Spectroscopy ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
Coordination Polymers ◽  
Elemental Analysis ◽  
Metal Organic Frameworks ◽  
X Ray Diffraction ◽  
Phase Purity ◽  
X Ray ◽  
Metal Organic

Abstract Three new metal−organic frameworks based on scandium(III) cations and 2,5-thiophenedicarboxylic acid (H2Tdc) are synthesized: [Sc(Tdc)(OH)]·1.2DMF (I), [Sc(Tdc)(OH)]·2/3DMF (II), and (Me2NH2)[Sc3(Tdc)4(OH)2]·DMF (III) (DMF is N,N-dimethylformamide). The structures of the compounds are determined by single-crystal X-ray structure analysis (CIF file CCDC nos. 2067819 (I), 2067820 (II), and 2067821 (III)). The chemical and phase purity of compound I is proved by elemental analysis, thermogravimetry, X-ray diffraction analysis, and IR spectroscopy.

scholarly journals Synthesis, Crystal Structure and Magnetic Behaviour of Novel 4f-2s Heterometalic One-Dimensional Coordination Polymers on the Base of 2-Furan-Carboxylic Acid

2009 ◽  
Vol 4 (2) ◽  
pp. 60-67
Author(s):  
Silvia Melnic ◽  
Denis Prodius ◽  
Sergiu Shova ◽  
Helen Stoeckli-Evans ◽  
Yurii Simonov ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Carboxylic Acid ◽  
Ir Spectra ◽  
Single Crystal ◽  
General Formula ◽  
Coordination Polymers ◽  
Magnetic Behaviour ◽  
One Dimensional ◽  
X Ray

Nine new complexes with the general formula {[Ln2Ba(α-Fur)8(H2O)4]}n, where Ln = Nd3+, Sm3+, Eu3+, Pr3+, Gd3+, Tb3+, Ho3+, Er3+ and La3+; α-Fur ≡ C4H3OCOO, were synthesized and characterized by IR spectra, magnetism, X-ray single crystal and powder diffractions.

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