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.

Two new CdII MOFs of 1,4-bis(1H-benzimidazol-1-yl)butane and flexible dicarboxylate ligands: luminescence sensing towards Fe3+

2020 ◽  
Vol 76 (11) ◽  
pp. 1024-1033
Author(s):  
Fang-Hua Zhao ◽  
Shi-Yao Li ◽  
Wen-Yu Guo ◽  
Zi-Hao Zhao ◽  
Xiao-Wen Guo ◽  
...  
Keyword(s):  
Aqueous Solution ◽  
Solid State ◽  
Hydrogen Bonds ◽  
Layer Structure ◽  
Three Dimensional ◽  
Supramolecular Network ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
Vis Spectroscopy

Two new CdII MOFs, namely, two-dimensional (2D) poly[[[μ2-1,4-bis(1H-benzimidazol-1-yl)butane](μ2-heptanedioato)cadmium(II)] tetrahydrate], {[Cd(C7H10O4)(C18H18N4)]·4H2O} n or {[Cd(Pim)(bbimb)]·4H2O} n (1), and 2D poly[diaqua[μ2-1,4-bis(1H-benzimidazol-1-yl)butane](μ4-decanedioato)(μ2-decanedioato)dicadmium(II)], [Cd2(C10H16O4)2(C18H18N4)(H2O)2] n or [Cd(Seb)(bbimb)0.5(H2O)] n (2), have been synthesized hydrothermally based on the 1,4-bis(1H-benzimidazol-1-yl)butane (bbimb) and pimelate (Pim2−, heptanedioate) or sebacate (Seb2−, decanedioate) ligands. Both MOFs were structurally characterized by single-crystal X-ray diffraction. In 1, the CdII centres are connected by bbimb and Pim2− ligands to generate a 2D sql layer structure with an octameric (H2O)8 water cluster. The 2D layers are further connected by O—H...O hydrogen bonds, resulting in a three-dimensional (3D) supramolecular structure. In 2, the CdII centres are coordinated by Seb2− ligands to form binuclear Cd2 units which are linked by bbimb and Seb2− ligands into a 2D hxl layer. The 2D layers are further connected by O—H...O hydrogen bonds, leading to an 8-connected 3D hex supramolecular network. IR and UV–Vis spectroscopy, thermogravimetric analysis and solid-state photoluminescence analysis were carried out on both MOFs. Luminescence sensing experiments reveal that both MOFs have good selective sensing towards Fe3+ in aqueous solution.

Self-Assembly of a Three-Dimensional Supramolecular Structure Based on Carboxyl-Bridged Tetrameric Water Clusters

2008 ◽  
Vol 2008 (10) ◽  
pp. 584-586 ◽  
Author(s):  
Fayan Meng ◽  
Yuanhong Jiao ◽  
Xuemei Chen ◽  
Lei Teng
Keyword(s):  
Thermogravimetric Analysis ◽  
Hydrogen Bonds ◽  
Water Loss ◽  
Self Assembly ◽  
Water Cluster ◽  
Room Temperature ◽  
Water Clusters ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
X Ray

A self-assembled, tetrameric water cluster stabilised by carboxyl-bridging has been characterised by X-ray diffraction studies and thermogravimetric analysis. Every water cluster is connected strongly via hydrogen bonds to four carboxyl oxygens of a terephthalate anion. The water rings are stable at room temperature, but when thermally decomposed, the water loss is irreversible.

scholarly journals Synthesis and physico-chemical studies of a novel coordination compound ZnCl2(C6H4FNH2)2

2014 ◽  
Vol 10 (3) ◽  
pp. 2502-2511 ◽  
Author(s):  
Mahjouba Ben Nasr ◽  
Emmanuel Aubert ◽  
Enrique Espinosa ◽  
Frederic Lefebvre ◽  
Cherif Ben Nasr
Keyword(s):  
Solid State ◽  
Hydrogen Bonds ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
Dimensional Network ◽  
Physico Chemical ◽  
Charge Transfer Transitions ◽  
Chemical Studies ◽  
Monodentate Ligands

A new Zn(II) complex with the monodentate ligand 3-fluoroaniline, ZnCl2(C6H4FNH2)2, has been prepared and characterized by single crystal X-ray diffraction, Solid state NMR, IR and UV-visible spectroscopies. The Zn(II) ion, located on a special position, is tetracoordinated by two nitrogen atoms of two 3-fluoroaniline monodentate ligands and two chlorine ligands. In the atomic arrangement, the ZnCl2(NH2)2 entities are interconnected via N-H…Cl hydrogen bonds to form inorganic layers parallel to the (b, c) plane. The organic 3-fluorophenyl groups are located between these layers and connect each other via C-H…F hydrogen bonds to perform an infinite three-dimensional network. The F atom of the 3-fluoroaniline ligand is disordered over two positions. An F-F interaction between neighboring fluorine atoms contributes also to the structure cohesion. The 13C and 15N CP-MAS NMR spectra are in agreement with the X-ray structure. DFT calculations allow the attribution of the carbon peaks to the different independent atoms. Solid-state UV-Vis spectrum of the complex has been assigned to ligand and charge transfer transitions.

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.

scholarly journals Acemetacin cocrystals and salts: structure solution from powder X-ray data and form selection of the piperazine salt

IUCrJ ◽  
2014 ◽  
Vol 1 (2) ◽  
pp. 136-150 ◽  
Author(s):  
Palash Sanphui ◽  
Geetha Bolla ◽  
Ashwini Nangia ◽  
Vladimir Chernyshev
Keyword(s):  
Hydrogen Bonds ◽  
Dissolution Rate ◽  
Aqueous Medium ◽  
Acid Amide ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
Reference Drug ◽  
X Ray ◽  
Time Period ◽  
Solid Form

Acemetacin (ACM) is a non-steroidal anti-inflammatory drug (NSAID), which causes reduced gastric damage compared with indomethacin. However, acemetacin has a tendency to form a less soluble hydrate in the aqueous medium. We noted difficulties in the preparation of cocrystals and salts of acemetacin by mechanochemical methods, because this drug tends to form a hydrate during any kind of solution-based processing. With the objective to discover a solid form of acemetacin that is stable in the aqueous medium, binary adducts were prepared by the melt method to avoid hydration. The coformers/salt formers reported are pyridine carboxamides [nicotinamide (NAM), isonicotinamide (INA), and picolinamide (PAM)], caprolactam (CPR),p-aminobenzoic acid (PABA), and piperazine (PPZ). The structures of an ACM–INA cocrystal and a binary adduct ACM–PABA were solved using single-crystal X-ray diffraction. Other ACM cocrystals, ACM–PAM and ACM–CPR, and the piperazine salt ACM–PPZ were solved from high-resolution powder X-ray diffraction data. The ACM–INA cocrystal is sustained by the acid...pyridine heterosynthon and N—H...O catemer hydrogen bonds involving the amide group. The acid...amide heterosynthon is present in the ACM–PAM cocrystal, while ACM–CPR contains carboxamide dimers of caprolactam along with acid–carbonyl (ACM) hydrogen bonds. The cocrystals ACM–INA, ACM–PAM and ACM–CPR are three-dimensional isostructural. The carboxyl...carboxyl synthon in ACM–PABA posed difficulty in assigning the position of the H atom, which may indicate proton disorder. In terms of stability, the salts were found to be relatively stable in pH 7 buffer medium over 24 h, but the cocrystals dissociated to give ACM hydrate during the same time period. The ACM–PPZ salt and ACM–nicotinamide cocrystal dissolve five times faster than the stable hydrate form, whereas the ACM–PABA adduct has 2.5 times faster dissolution rate. The pharmaceutically acceptable piperazine salt of acemetacin exhibits superior stability, faster dissolution rate and is able to overcome the hydration tendency of the reference drug.

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.

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.

Notizen: Solid State Structure of N,N-Dibenzylhydroxylamine

1995 ◽  
Vol 50 (4) ◽  
pp. 699-701 ◽  
Author(s):  
Norbert W. Mitzel ◽  
Jürgen Riede ◽  
Klaus Angermaier ◽  
Hubert Schmidbaur
Keyword(s):  
Solid State ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
State Structure ◽  
X Ray Diffraction ◽  
Space Group ◽  
Solid State Structure ◽  
X Ray

The solid-state structure of N,N-dibenzylhydroxylamine (1) has been determined by single crystal X-ray diffraction. The compound crystallizes in the monoclinic space group P 21/n with four formula units in the unit cell. N,N-dibenzylhydroxylamine dimerizes to give N2O2H2 sixmembered rings as a result of the formation of two hydrogen bonds O - H ··· N in the solid state.

A novel dinuclear bismuth(III) coordination compound: bis(μ-pyridine-2,6-dicarboxylato)-κ4O2,N,O6:O6′;κ4O2:O2′,N,O6-bis[(azido-κN)(1,10-phenanthroline-κ2N,N′)bismuth(III)] tetrahydrate

2014 ◽  
Vol 70 (6) ◽  
pp. 562-565 ◽  
Author(s):  
Wei Zhang ◽  
Yu-Quan Feng
Keyword(s):  
Molecular Structure ◽  
Hydrogen Bonds ◽  
Coordination Compound ◽  
Photoelectron Spectroscopy ◽  
Three Dimensional ◽  
Water Molecules ◽  
Stacking Interactions ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
X Ray

A novel dinuclear bismuth(III) coordination compound, [Bi2(C7H3NO4)2(N3)2(C12H8N2)2]·4H2O, has been synthesized by an ionothermal method and characterized by elemental analysis, energy-dispersive X-ray spectroscopy, IR, X-ray photoelectron spectroscopy and single-crystal X-ray diffraction. The molecular structure consists of one centrosymmetric dinuclear neutral fragment and four water molecules. Within the dinuclear fragment, each BiIIIcentre is seven-coordinated by three O atoms and four N atoms. The coordination geometry of each BiIIIatom is distorted pentagonal–bipyramidal (BiO3N4), with one azide N atom and one bridging carboxylate O atom located in axial positions. The carboxylate O atoms and water molecules are assembledviaO—H...O hydrogen bonds, resulting in the formation of a three-dimensional supramolecular structure. Two types of π–π stacking interactions are found, with centroid-to-centroid distances of 3.461 (4) and 3.641 (4) Å.

Sign in / Sign up

Export Citation Format

Share Document