Honeycomb molecular network based upon a hydrate of 4,6-dichlororesorcinol and the photoproduct rtct-tetrakis(pyridin-4-yl)cyclobutane

2021 ◽  
Vol 77 (2) ◽  
pp. 111-115
Author(s):  
Carlos L. Santana ◽  
Jessica D. Battle ◽  
Daniel K. Unruh ◽  
Ryan H. Groeneman
Keyword(s):  
Hydrogen Bonds ◽  
Water Molecule ◽  
Single Crystal ◽  
Organic Materials ◽  
Molecular Network ◽  
Molecular Solids ◽  
X Ray ◽  
Bridging Ligand ◽  
Metal Organic ◽  
Cyclobutane Ring

The formation of a self-interpenetrated honeycomb molecular network based upon 4,6-dichlororesorcinol (4,6-diCl res), a water molecule, and the photoproduct rtct-tetrakis(pyridin-4-yl)cyclobutane ( rtct -TPCB) is reported. Interestingly, only three of the four pyridine rings on the central cyclobutane ring are found to engage in O—H...N hydrogen bonds with either the 4,6-diCl res or an included water molecule, resulting in a three-connected net. Notably, the solid (4,6-diCl res)·( rtct -TPCB)·(H2O), C6H4Cl2O2·C24H20N4·H2O, contains channels that run along the crystallographic b axis, which are found to be interpenetrated. Although rtct -TPCB has been employed as a bridging ligand in the formation of numerous metal–organic materials, surprisingly neither the single-component X-ray structure nor any multi-component molecular solids based upon this stereoisomer have been reported previously. Lastly, the single-crystal X-ray structure of the photoproduct rtct -TPCB is also reported.

scholarly journals A new one-dimensional NiIIcoordination polymer with a two-dimensional supramolecular architecture

2017 ◽  
Vol 73 (2) ◽  
pp. 192-195
Author(s):  
Kai-Long Zhong
Keyword(s):  
Hydrogen Bonds ◽  
Water Molecule ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
Sulfate Ions ◽  
Sulfate Anion ◽  
One Dimensional ◽  
X Ray ◽  
Distorted Octahedral ◽  
Metal Organic

A new one-dimensional NiIIcoordination polymer of 1,3,5-tris(imidazol-1-ylmethyl)benzene, namelycatena-poly[[aqua(sulfato-κO)hemi(μ-ethane-1,2-diol-κ2O:O′)[μ3-1,3,5-tris(1H-imidazol-1-ylmethyl)benzene-κ3N3,N3′,N3′′]nickel(II)] ethane-1,2-diol monosolvate monohydrate], {[Ni(SO4)(C18H18N6)(C2H6O2)0.5(H2O)]·C2H6O2·H2O}n, was synthesized and characterized by elemental analysis, IR spectroscopy and single-crystal X-ray diffraction. The NiIIcation is coordinated by three N atoms of three different 1,3,5-tris(imidazol-1-ylmethyl)benzene ligands, one O atom of an ethane-1,2-diol molecule, by a sulfate anion and a water molecule, forming a distorted octahedral NiN3O3coordination geometry. The tripodal 1,3,5-tris(imidazol-1-ylmethyl)benzene ligands link the NiIIcations, generating metal–organic chains running along the [100] direction. Adjacent chains are further connected by O—H...O hydrogen bonds, resulting in a two-dimensional supermolecular architecture running parallel to the (001) plane. Another water molecule and a second ethane-1,2-diol molecule are non-coordinating and are linked to the coordinating sulfate ionsviaO—H...O hydrogen bonds.

scholarly journals Thermal Reactivity in Metal Organic Materials (MOMs): From Single-Crystal-to-Single-Crystal Reactions and Beyond

Materials ◽  
2019 ◽  
Vol 12 (24) ◽  
pp. 4088
Author(s):  
Javier Martí-Rujas
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Organic Materials ◽  
Structural Transformations ◽  
Atomic Motion ◽  
X Ray Diffraction ◽  
Thermally Induced ◽  
X Ray ◽  
Thermal Reactivity ◽  
Metal Organic

Thermal treatment is important in the solid-state chemistry of metal organic materials (MOMs) because it can create unexpected new structures with unique properties and applications that otherwise in the solution state are very difficult or impossible to achieve. Additionally, high-temperature solid-state reactivity provide insights to better understand chemical processes taking place in the solid-state. This review article describes relevant thermally induced solid-state reactions in metal organic materials, which include metal organic frameworks (MOFs)/coordination polymers (CPs), and second coordination sphere adducts (SSCs). High temperature solid-state reactivity can occur in a single-crystal-to-single crystal manner (SCSC) usually for cases where there is small atomic motion, allowing full structural characterization by single crystal X-ray diffraction (SC-XRD) analysis. However, for the cases in which the structural transformations are severe, often the crystallinity of the metal-organic material is damaged, and this happens in a crystal-to-polycrystalline manner. For such cases, in the absence of suitable single crystals, structural characterization has to be carried out using ab initio powder X-ray diffraction analysis or pair distribution function (PDF) analysis when the product is amorphous. In this article, relevant thermally induced SCSC reactions and crystal-to-polycrystalline reactions in MOMs that involve significant structural transformations as a result of the molecular/atomic motion are described. Thermal reactivity focusing on cleavage and formation of coordination and covalent bonds, crystalline-to-amorphous-to-crystalline transformations, host–guest behavior and dehydrochlorination reactions in MOFs and SSCs will be discussed.

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

Single Crystal X-ray Diffraction Studies of Carbon Dioxide and Fuel-Related Gases Adsorbed on the Small Pore Scandium Terephthalate Metal Organic Framework, Sc2(O2CC6H4CO2)3

Langmuir ◽  
2009 ◽  
Vol 25 (6) ◽  
pp. 3618-3626 ◽  
Author(s):  
Stuart R. Miller ◽  
Paul A. Wright ◽  
Thomas Devic ◽  
Christian Serre ◽  
Gérard Férey ◽  
...  
Keyword(s):  
Carbon Dioxide ◽  
Single Crystal ◽  
Metal Organic Framework ◽  
X Ray Diffraction ◽  
X Ray ◽  
Small Pore ◽  
Metal Organic ◽  
Organic Framework

A series of microporous and robust Ln-MOFs showing luminescent properties and catalytic performances towards Knoevenagel reactions

2021 ◽  
Author(s):  
Qing-Xia Yao ◽  
Miaomiao Tian ◽  
Jun Zheng ◽  
Jintang Xue ◽  
Xuze Pan ◽  
...  
Keyword(s):  
Single Crystal ◽  
Metal Organic Frameworks ◽  
Luminescent Properties ◽  
X Ray Diffraction ◽  
X Ray ◽  
Metal Organic ◽  
Catalytic Performances

A series of microporous Ln(III)-based metal-organic frameworks (1-Ln) have been hydrothermally synthesized by using 4,4',4''-nitrilotribenzoic acid (H3NTB). Single crystal X-ray diffraction analyses show 1-Ln are isostructural and have 3D porous...

Thermal-induced transformation of glutamic acid to pyroglutamic acid and self-cocrystallization: a charge–density analysis

2022 ◽  
Vol 78 (2) ◽  
Author(s):  
Sehrish Akram ◽  
Arshad Mehmood ◽  
Sajida Noureen ◽  
Maqsood Ahmed
Keyword(s):  
Hydrogen Bonds ◽  
Glutamic Acid ◽  
Single Crystal ◽  
Diffraction Data ◽  
Density Functional ◽  
Quantitative Estimation ◽  
Topological Analysis ◽  
Pyroglutamic Acid ◽  
X Ray Diffraction ◽  
X Ray

Thermal-induced transformation of glutamic acid to pyroglutamic acid is well known. However, confusion remains over the exact temperature at which this happens. Moreover, no diffraction data are available to support the transition. In this article, we make a systematic investigation involving thermal analysis, hot-stage microscopy and single-crystal X-ray diffraction to study a one-pot thermal transition of glutamic acid to pyroglutamic acid and subsequent self-cocrystallization between the product (hydrated pyroglutamic acid) and the unreacted precursor (glutamic acid). The melt upon cooling gave a robust cocrystal, namely, glutamic acid–pyroglutamic acid–water (1/1/1), C5H7NO3·C5H9NO4·H2O, whose structure has been elucidated from single-crystal X-ray diffraction data collected at room temperature. A three-dimensional network of strong hydrogen bonds has been found. A Hirshfeld surface analysis was carried out to make a quantitative estimation of the intermolecular interactions. In order to gain insight into the strength and stability of the cocrystal, the transferability principle was utilized to make a topological analysis and to study the electron-density-derived properties. The transferred model has been found to be superior to the classical independent atom model (IAM). The experimental results have been compared with results from a multipolar refinement carried out using theoretical structure factors generated from density functional theory (DFT) calculations. Very strong classical hydrogen bonds drive the cocrystallization and lend stability to the resulting cocrystal. Important conclusions have been drawn about this transition.

A Mn(II) Metal-Organic Framework Constructed from a Tetrahedral Silicon-Cored Ligand

2013 ◽  
Vol 275-277 ◽  
pp. 2367-2370
Author(s):  
Qing Yu Ma ◽  
Rui Fang Guan ◽  
Guo Zhong Li ◽  
Deng Xu Wang
Keyword(s):  
Single Crystal ◽  
Metal Organic Framework ◽  
Diffusion Method ◽  
X Ray Diffraction ◽  
X Ray ◽  
Slow Diffusion ◽  
Sheet Structure ◽  
Metal Organic ◽  
1D Chains ◽  
Organic Framework

A novel metal-organic framework, MnCl2(BIPS)2•2CH3OH•2H2O (1) were synthesized from MnCl2 and a tetrahedral silicon-cored ligand, Me2Si(p-C6H4-imdazol-1-yl)2 (BIPS) under the slow diffusion method. The structure was determined by single-crystal X-ray diffraction. Complex 1 is a 2D sheet structure constructed from 1D chains with 34-atom metallamacrocycles.

scholarly journals Crystal structure of tris(pyridine)(salicylaldehyde semicarbazonato(2-))cobalt(III)-trichloropyridinecobaltate(II) at 293 and 120K

2007 ◽  
Vol 72 (1) ◽  
pp. 63-71 ◽  
Author(s):  
Goran Bogdanovic ◽  
Vukadin Leovac ◽  
Ljiljana Vojinovic-Jesic ◽  
Biré-Spasojevic De
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Intermolecular Interaction ◽  
Complex Anion ◽  
Octahedral Geometry ◽  
Pyridine Ligand ◽  
Similar Composition ◽  
X Ray ◽  
Preferential Position

The crystal structure of [CoIII(L)(py)3][CoIICl3(py)] (H2L=salicylaldehyde semicarbazone)was determined by X-ray analysis based on two single crystal X-ray experiments performed at 120 K and 293 K, respectively. It was found that the pyridine ligand of the complex anion is disordered over two positions. The preferential position of this pyridine found at120Kwas explained in terms of the C-H...Cl intermolecular interaction between the tetrahedral [CoII(py)Cl3]- anions. The mer-octahedral geometry of the cation in the presented crystal structure was compared with previously published structures of similar composition, [CoIII(L1)(py)3]+[CoIICl3(py)]-?EtOH and [CoIII(LI)(py)3]+I3-(H2LI = salicylaldehyde S-methylisothiosemicarbazone). Although the tetrahedral [CoIICl3(py)]- anions possess the same charge, they mutually form different intermolecular interactions which can be realized either by C-H...Cl hydrogen bonds or by ?-? interactions between the pyridine rings.

Crystal Structure of Calcium Picrate Pentahydrate: A New Eight-Coordinate Stereochemistry for [M(bidentate)2(unidentate)4]

1979 ◽  
Vol 32 (2) ◽  
pp. 301 ◽  
Author(s):  
V Diakiw ◽  
TW Hambley ◽  
DL Kepert ◽  
CL Raston ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Water Molecule ◽  
Single Crystal ◽  
Title Compound ◽  
Lattice Site ◽  
The Other ◽  
Water Molecules ◽  
X Ray Diffraction ◽  
Triangular Face ◽  
X Ray

The crystal structure of the title compound, Ca(C6H2N307)2,5H2O, has been determined by single-crystal X-ray diffraction at 295(1) K and refined by least squares to a residual of 0.049 for 1513 'observed' reflections. Crystals are orthorhombic, Pmab, a 24.169(6), b l0.292(7), c 8.554(2) �, Z 4. The stereochemistry about the calcium has not been observed previously for the system [M(bidentate)2- (unidentate)4]; in the present structure, the calcium is coordinated by a pair of bidentate picrate ligands and the four water molecules in an array in which three of the water molecules occupy a triangular face of a square antiprism, the overall array having m symmetry. The remaining water molecule occupies a lattice site with no close interaction with the other species.

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