scholarly journals Crystal Structure and Computational Study on Methyl-3-Aminothiophene-2-Carboxylate

Crystals ◽  
2020 ◽  
Vol 10 (1) ◽  
pp. 19 ◽  
Author(s):  
Yaping Tao ◽  
Ligang Han ◽  
Andong Sun ◽  
Kexi Sun ◽  
Qian Zhang ◽  
...  
Keyword(s):  
Crystal Packing ◽  
Computational Study ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
Dispersion Energy ◽  
Monoclinic Crystal ◽  
Hydrogen Bond Interactions ◽  
Calculation Results ◽  
Reduced Density Gradient ◽  
Reduced Density

Methyl-3-aminothiophene-2-carboxylate (matc) is a key intermediate in organic synthesis, medicine, dyes, and pesticides. Single crystal X-ray diffraction analysis reveals that matc crystallizes in the monoclinic crystal system P21/c space group. Three matc molecules in the symmetric unit are crystallographically different and further linked through the N–H⋯O and N–H⋯N hydrogen bond interactions along with weak C–H⋯S and C–H⋯Cg interactions, which is verified by the three-dimensional Hirshfeld surface, two-dimensional fingerprint plot, and reduced density gradient (RDG) analysis. The interaction energies within crystal packing are visualized through dispersion, electrostatic, and total energies using three-dimensional energy-framework analyses. The dispersion energy dominates in crystal packing. To better understand the properties of matc, electrostatic potential (ESP) and frontier molecular orbitals (FMO) were also calculated and discussed. Experimental and calculation results suggested that amino and carboxyl groups can participate in various inter- and intra-interactions.

Theoretical and experimental solid state studies of Ethyl 1-benzyl-2-(thiophen-3-yl)-1H-benzo[d]imidazole-5-carboxylate

2020 ◽  
Vol 235 (11) ◽  
pp. 569-579
Author(s):  
Shankar Madan Kumar ◽  
Vasantha Kumar ◽  
Mohammed Al-Ghorbani ◽  
Bantwala Shivaram Holla ◽  
Boja Poojary ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Crystal Packing ◽  
Three Dimensional ◽  
Diffraction Method ◽  
Band Gap Energy ◽  
Electrostatic Energy ◽  
Energy Term ◽  
X Ray Diffraction ◽  
Dispersion Energy ◽  
Intermolecular Contacts

AbstractThe title compound Ethyl 1-benzyl-2-(thiophen-3-yl)-1H-benzo[d]imidazole-5-carboxylate (BI) is prepared and characterized using spectroscopic methods. The theoretical optimization and three dimensional molecular structure are confirmed by X-ray diffraction method (single crystal). The C–H…π intermolecular interactions stabilize the crystal structure. The intermolecular contacts in the crystal structure are quantified using Hirshfeld surfaces and the crystal packing is elucidated using 3D energy frameworks analysis. In the frameworks, the dispersion energy term is dominated over the electrostatic energy term. The structural optimization was carried out with B3LYP/6-311++G (d, p) level of theory. The visual representations of positive and negative potentials (electrostatic potential) are mapped on the electron density isosurface. The band gap energy (HOMO-LUMO) of the molecule is calculated to be 4.36 eV. Structural conformation of BI is compared with similar structures.

scholarly journals Synthesis, Spectral, Structural and Thermal Characterization of Inorganic Crystal: Phenyl Trimethylammonium Tetrachlorocobaltate

2019 ◽  
Vol 31 (8) ◽  
pp. 1779-1784
Author(s):  
V. Mohanraj ◽  
R. Pavithra ◽  
M. Thenmozhi ◽  
R. Umarani
Keyword(s):  
Three Dimensional ◽  
Thermal Characterization ◽  
Dimensional Structure ◽  
X Ray Diffraction ◽  
Monoclinic Crystal ◽  
Evaporation Technique ◽  
Ft Ir ◽  
Thermal Stability Of ◽  
Ft Ir Spectroscopy

Phenyl trimethylammonium tetrachlorocobaltate, crystals were grown by slow evaporation technique. The crystal was bright, transparent. The three dimensional structure of the phenyl trimethylammonium tetrachlorocobaltate was obtained from single crystal X-ray diffraction studies. The molecule belongs to monoclinic crystal system with C2/c space group. The presence of functional groups and modes of vibrations were identified by FT-IR spectroscopy. 1H NMR spectroscopy was also used to characterise the compound and the thermal stability of the crystal was established by TGA/DT analysis. This work undergoes phase transition which makes the study interesting.

scholarly journals NMR crystallography, diffraction and modeling of small organic molecules

2014 ◽  
Vol 70 (a1) ◽  
pp. C1088-C1088
Author(s):  
Luís Miguel Monteiro Mafra
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Crystal Packing ◽  
Computational Study ◽  
Chemical Shifts ◽  
Hybrid Approach ◽  
X Ray Diffraction ◽  
Structure Solution ◽  
Nmr Crystallography

Solid-state NMR (SSNMR) is a powerful atomic-level characterization technique able to study the local chemical environment of a nucleus in crystalline/amorphous solids. Toward a better understanding of how small molecules self-assemble in the solid-state and reorganizes to produce its hydrate/anhydrous forms, an experimental SSNMR, X-ray diffraction (XRD), and computational study of the supramolecular assemblies of selected small pharmaceuticals is presented. The effect of crystal packing on the 1H and 13C chemical shifts including nonconventional hydrogen bonds, pi···pi and CH···pi contacts, is studied through computer simulations. It will be shown that NMR chemical shifts are sensitive detectors of hydration/dehydration states in highly insoluble antibiotics.[1] Recently, SSNMR became an important gadget in the process of crystal structure solution in powders. This is a non-trivial task and using powder XRD methods alone may often lead to the wrong structure solution. In this talk, a new hybrid approach for structure determination of crystalline solids, will be presented, based on the combination of SSNMR, XRD and an ensemble of computational-assisted structure solution tools including a genetic algorithm based on evolution-inspired operators repeatedly applied to populations of possible crystal structure solutions that evolve to eventually produce the best new offspring candidates. Such methodologies are successfully applied to challenging cases involving multiple component crystals composed by flexible molecules such as a trihydrate β-lactamic antibiotic [2] and an azole-based co-crystal featuring an hydrogen bond network of α-helixes involving NH···N/CH···π intermolecular interactions. ACKNOLEDGEMENTS: Supported by Fundação para a Ciência e a Tecnologia (FCT), Portuguese National NMR Network (RNRMN), CICECO (PEst-C/CTM/LA0011/2013), FEDER, COMPETE, and University of Aveiro. FCT is greatly acknowledge for the consolidation grant IF/01401/2013.

Synthesis, Crystal Structure, and Theoretical Calculations of Two Cobalt, Nickel Coordination Polymers with 5-Nitroisophthalic Acid and Bis(imidazol) Ligands

2016 ◽  
Vol 69 (11) ◽  
pp. 1296 ◽  
Author(s):  
Ya-Ru Pan ◽  
Xiu-Mei Li ◽  
Jian-Ye Ji ◽  
Qing-Wei Wang
Keyword(s):  
Theoretical Calculations ◽  
Uv Spectroscopy ◽  
Three Dimensional ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
Cobalt Nickel ◽  
Hydrogen Bonding Interactions ◽  
Calculation Results ◽  
Covalent Interactions ◽  
2D Network

Two new complexes [Co(NIPH)(bimb)(H2O)]n (1) and [Ni(NIPH)(mbix)]n (2) (H2NIPH = 5-nitroisophthalic acid, bimb = 1,4-bis(imidazol-1-yl)butane, mbix = 1,3-bis(imidazol-1-ylmethyl)benzene) have been hydrothermally synthesised and structurally characterised by elemental analysis, IR spectroscopy, thermogravimetric analysis, UV spectroscopy, and single-crystal X-ray diffraction. Complex 1 exhibits a two-dimensional (2D) network, which was stabilised through O–H···O and C–H···O hydrogen-bonding interactions. Complex 2 shows a two-dimensional (2D) network structure, which was further extended into a three-dimensional supramolecular structure through C–H···O hydrogen bonds and π–π interactions. Moreover, we analysed the natural bond orbital (NBO) using the PBE0/LANL2DZ method in the Gaussian 03 program. The calculation results indicated the obvious covalent interactions between the coordinated atoms and the CoII or NiII ion.

A new three-dimensional CdIIsupramolecular framework constructed from the 1-[(1H-tetrazol-5-yl)methyl]-1,4-diazoniabicyclo[2.2.2]octane ligand

2015 ◽  
Vol 71 (2) ◽  
pp. 93-96 ◽  
Author(s):  
Qiang Li ◽  
Hui-Ting Wang ◽  
Lin Zhou
Keyword(s):  
Crystal Packing ◽  
Three Dimensional ◽  
Supramolecular Network ◽  
Stacking Interactions ◽  
X Ray Diffraction ◽  
One Dimensional ◽  
X Ray ◽  
Distorted Octahedral Coordination Geometry ◽  
Distorted Octahedral ◽  
Cl Atoms

A new tetrazole–metal supramolecular compound, di-μ-chlorido-bis(trichlorido{1-[(1H-tetrazol-5-yl-κN2)methyl]-1,4-diazoniabicyclo[2.2.2]octane}cadmium(II)), [Cd2(C8H16N6)2Cl8], has been synthesized and structurally characterized by single-crystal X-ray diffraction. In the structure, each CdIIcation is coordinated by five Cl atoms (two bridging and three terminal) and by one N atom from the 1-[(1H-tetrazol-5-yl)methyl]-1,4-diazoniabicyclo[2.2.2]octane ligand, adopting a slightly distorted octahedral coordination geometry. The bridging bicyclo[2.2.2]octane and chloride ligands link the CdIIcations into one-dimensional ribbon-like N—H...Cl hydrogen-bonded chains along thebaxis. An extensive hydrogen-bonding network formed by N—H...Cl and C—H...Cl hydrogen bonds, and interchain π–π stacking interactions between adjacent tetrazole rings, consolidate the crystal packing, linking the poymeric chains into a three-dimensional supramolecular network.

Study on Novel Structure of Potassium Borate Hydrate: K(H4B5O10)·2(H2O)

2012 ◽  
Vol 531-532 ◽  
pp. 409-412
Author(s):  
Hai Xing Liu ◽  
Fang Fang Jian ◽  
Jing Wang ◽  
Guang Zeng ◽  
Hui Juan Yue ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Crystal Packing ◽  
Three Dimensional ◽  
Crystallographic Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Potassium Borate ◽  
Polyhydroxy Compounds ◽  
Novel Structure ◽  
Solution Reaction

Numerous stable complexes of boric acid with polyhydroxy compounds, including tartaric, salicylic, citric, malic, and other acids, are known. The structure of some compounds contains polyanion. In this paper, a novel potassium borate hydrate [K(H4B5O10) •2(H2O)] has been synthesized from a solution reaction and the crystal structure has been determined by means of single-crystal X-ray diffraction. Orthorhombic, Aba2. a = 11.0781(14) Å b = 11.1780(15) Å c = 9.0508(11) Å α=β=γ=90°. V= 1120.8(2) Å3. Z=4. Rgt = 0.0244, wRref = 0.0623. T= 298 K. The crystal packing is stabilized by O-H...O hydrogen bonds interaction and three dimensional framwork structure is formed. The work is originality and has a new crystallographic structure shape.

A two-dimensional copper(II) coordination polymer based on 2-propyl-1H-imidazole-4,5-dicarboxylic acid

2015 ◽  
Vol 71 (2) ◽  
pp. 152-154 ◽  
Author(s):  
Di-Chang Zhong ◽  
Hua-Bin Guo ◽  
Ji-Hua Deng ◽  
Ping Lian ◽  
Xu-Zhong Luo
Keyword(s):  
Hydrogen Bond ◽  
Carboxylic Acid ◽  
Dicarboxylic Acid ◽  
Three Dimensional ◽  
Acid Group ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
Carboxylic Acid Group ◽  
X Ray ◽  
Hydrogen Bond Interactions

Single-crystal X-ray diffraction analysis of poly[bis(μ2-5-carboxy-2-propyl-1H-imidazole-4-carboxylato-κ3N3,O4:O5)copper(II)], [Cu(C8H9N2O4)2)]n, indicates that one carboxylic acid group of the 2-propyl-1H-imidazole-4,5-dicarboxylic acid (H3PDI) ligand is deprotonated. The resulting H2PDI−anion, acting as a bridge, connects the CuIIcations to form a two-dimensional (4,4)-connected layer. Adjacent layers are further linked through interlayer hydrogen-bond interactions, resulting in a three-dimensional supramolecular structure.

A complementary experimental and computational study of loxapine succinate and its monohydrate

2013 ◽  
Vol 69 (11) ◽  
pp. 1273-1278 ◽  
Author(s):  
Rajni M. Bhardwaj ◽  
Blair F. Johnston ◽  
Iain D. H. Oswald ◽  
Alastair J. Florence
Keyword(s):  
Succinic Acid ◽  
Powder Diffraction ◽  
Density Functional ◽  
Crystal Packing ◽  
Computational Study ◽  
Geometry Optimization ◽  
Global Optimum ◽  
X Ray Diffraction ◽  
X Ray ◽  
Fixed Cell

The crystal structures of loxapine succinate [systematic name: 4-(2-chlorodibenzo[b,f][1,4]oxazepin-11-yl)-1-methylpiperazin-1-ium 3-carboxypropanoate], C18H19ClN3O+·C4H5O4−, and loxapine succinate monohydrate {systematic name: bis[4-(2-chlorodibenzo[b,f][1,4]oxazepin-11-yl)-1-methylpiperazin-1-ium] succinate succinic acid dihydrate}, 2C18H19ClN3O+·C4H4O42−·C4H6O4·2H2O, have been determined using X-ray powder diffraction and single-crystal X-ray diffraction, respectively. Fixed cell geometry optimization calculations using density functional theory confirmed that the global optimum powder diffraction derived structure also matches an energy minimum structure. The energy calculations proved to be an effective tool in locating the positions of the H atoms reliably and verifying the salt configuration of the structure determined from powder data. Crystal packing analysis of these structures revealed that the loxapine succinate structure is based on chains of protonated loxapine molecules while the monohydrate contains dispersion stabilized centrosymmetric dimers. Incorporation of water molecules within the crystal lattice significantly alters the molecular packing and protonation state of the succinic acid.

scholarly journals Substituent Effect on AIE Mechanism of Two Coumarin Derivatives: Uncommon TICT Fluorescence in Aggregation State

2022 ◽  
Author(s):  
Qiao Li ◽  
Yang Zhao ◽  
Zhigang Niu ◽  
Enju Wang
Keyword(s):  
Intramolecular Charge Transfer ◽  
Knoevenagel Condensation ◽  
Crystal Packing ◽  
Coumarin Derivatives ◽  
Dual Fluorescence ◽  
X Ray Diffraction ◽  
Aggregation State ◽  
X Ray ◽  
Hydrogen Bond Interactions ◽  
Salicylaldehyde Derivatives

Abstract Two coumarin derivatives, 7-diethylamino-3-(4-nitrophenyl)coumarin (DNC) and 7-hydroxy-3-(4-nitrophenyl)coumarin (HNC), were synthesized via Knoevenagel condensation of salicylaldehyde derivatives with 4-nitrophenylacetonitrile and then cyclization reaction. Both of them were characterized by single-crystal X-ray diffraction. The molecules of DNC are stacked via π-π interaction, while the hydrogen bond interactions instead of π-π interaction were observed in the crystal packing of HNC. Both of DNC and HNC showed solvatochromic properties and aggregation-induced emission (AIE) activities, but the AIE characteristics of them were entirely different. HNC exhibited an AIE phenomenon as the result of the restriction of twisted intramolecular charge transfer (TICT), while DNC emited peculiar dual fluorescence which was assigned to the emission based on the inhibition of TICT state formation and the emission from the TICT state respectively.

Dinuclear cobalt and nickel complexes of a mercaptoacetic acid substituted 1,2,4-triazole ligand: syntheses, structures and urease inhibitory studies

2019 ◽  
Vol 75 (12) ◽  
pp. 1658-1665 ◽  
Author(s):  
Zi-Yi Fang ◽  
Li Zhang ◽  
Jian-Ping Ma ◽  
Long Zhao ◽  
Shi-Ling Wang ◽  
...  
Keyword(s):  
Three Dimensional ◽  
Mercaptoacetic Acid ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
Hydrogen Bond Interactions ◽  
Triazole Ligand ◽  
Coordination Ability ◽  
Urease Inhibitory ◽  
Cobalt And Nickel

Because of its versatile coordination modes and strong coordination ability, the mercaptoacetic acid substituted 1,2,4-triazole 2-{[5-(pyridin-2-yl)-4H-1,2,4-triazol-3-yl]sulfanyl}acetic acid (H2L) was synthesized and characterized. Treatment of H2L with cobalt and nickel acetate afforded the dinuclear complexes {μ-3-[(carboxylatomethyl)sulfanyl]-5-(pyridin-2-yl)-4H-1,2,4-triazol-4-ido-κ2 N 1,N 5:N 2,O}bis[aqua(methanol-κO)cobalt(II)] methanol disolvate, [Co2(C9H6N4O2S)2(CH3OH)2(H2O)2]·2CH3OH (1), and {μ-3-[(carboxylatomethyl)sulfanyl]-5-(pyridin-2-yl)-4H-1,2,4-triazol-4-ido-κ2 N 1,N 5:N 2,O}bis[diaquanickel(II)] methanol disolvate dihydrate, [Ni2(C9H6N4O2S)2(H2O)4]·2CH3OH·2H2O (2), respectively. Complex 1 crystallized in the monoclinic space group P21/c, while 2 crystallized in the tetragonal space group I41/a. Single-crystal X-ray diffraction studies revealed that H2L is doubly deprotonated and acts as a tetradentate bridging ligand in complexes 1 and 2. For both of the obtained complexes, extensive hydrogen-bond interactions contribute to the formation of their three-dimensional supermolecular structures. Hirshfeld surface analysis was used to illustrate the intermolecular interactions. Additionally, the urease inhibitory activities of 1, 2 and H2L were investigated against jack bean urease, where the two complexes revealed strong urease inhibition activities.

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