Search results for "Hirshfeld"
showing 10 items of 69 documents
Synthesis and X-ray Crystal Structure Analysis of Substituted 1,2,4-Triazolo [4’,3’:2,3]pyridazino[4,5-b]indole and Its Precursor
2023
The hit compound 1,2,4-triazolo[4’,3’:2,3]pyridazino[4,5-b]indole 3 was synthesized from the reflux of 4-amino-5-indolyl-1,2,4-triazole-3-thione 1 with 4′-bromoacetophenone 2 in methanol catalyzed by concentrated HCl and the desired final molecule was obtained by recrystallization from methanol. The suggested structures of compounds 1 and 3 based on the spectral characterizations were confirmed by X-ray single crystal diffraction analysis. Compound 3 crystallized in the triclinic crystal system and P-1 space group with a = 5.9308(2) Å, b = 10.9695(3) Å, c = 14.7966(4) Å, α = 100.5010(10)°, β = 98.6180(10)°, and γ = 103.8180(10)°. On the other hand, the crystal system of 1 is monoclinic, whe…
Temperature-dependent polymorphism of N-(4-fluorophenyl)-1,5-dimethyl-1H-imidazole-4-carboxamide 3-oxide: experimental and theoretical studies on int…
2014
X-ray analysis of N-(4-fluorophenyl)-1,5-dimethyl-1H-imidazole-4-carboxamide 3-oxide reveals the temperature-dependent polymorphism associated with the crystallographic symmetry conversion. The observed crystal structure transformation corresponds to a symmetry reduction from I41 /a (I) to P43 (II) space groups. The phase transition mainly concerns the subtle but clearly noticeable reorganization of molecules in the crystal space, with the structure of individual molecules left almost unchanged. The Hirshfeld surface analysis shows that various intermolecular contacts play an important role in the crystal packing, revealing graphically the differences in spatial arrangements of the molecule…
Straightforward One-Pot Synthesis of New 4-Phenyl-1,2,5,6-tetraazafluoranthen-3(2H)-one Derivatives: X-ray Single Crystal Structure and Hirshfeld Ana…
2022
A straightforward one-pot route for the synthesis of a new 4-phenyl-1,2,5,6-tetraazafluoranthen-3(2H)-one is reported form the direct hydrazinolysis of triketo ester and hydrazine hydrate in ethanol. 4-Phenyl-1,2,5,6-tetraazafluoranthen-3(2H)-one was subjected to aza-Michael addition and N-alkylation on reaction with a set of alkylating agents in the presence of K2CO3. Hydrazinolysis of 4-phenyl-1,2,5,6-tetraazafluoranthen-3(2H)-one ester to hydrazide and conversion of hydrazide to thiosemicarbazide were successful. X-Ray single crystals analysis and 1H, 13C NMR were used for unambiguous structure confirmation. The O…H, N…H, C…N and C…C in 2, and the N…H, …
Synthesis, X-ray Structure of Two Hexa-Coordinated Ni(II) Complexes with s-Triazine Hydrazine Schiff Base Ligand
2023
The hydrazine s-triazine ligand (E)-4,4’-(6-(2-(1-(pyridin-2-yl)ethylidene)hydrazinyl)-1,3,5-triazine-2,4-diyl)dimorpholine (DMPT) was used to synthesize two new Ni(II) complexes via a self-assembly technique. The two complexes were synthesized by a one-pot synthesis strategy and characterized by elemental analysis, FTIR and single-crystal X-ray diffraction analysis to be [Ni(DMPT)(H2O)3](NO3)2.3H2O (1) and [Ni(DMPT)(H2O)3](NO3)2.H2O (2). The structures of both complexes were very similar regarding the coordination sphere and counter anions, but differ only in the number of the crystal water molecules. In the case of complex 1, there are three water molecules instead of one H2O molecu…
Synthesis and Characterizations of Novel Isatin-s-Triazine Hydrazone Derivatives : X-ray Structure, Hirshfeld Analysis and DFT Calculations
2023
A novel series of isatin-s-triazine hydrazone derivatives has been synthesized and reported herein. The synthetic methodology involved the reaction of s-triazine hydrazine precursors with isatin derivatives in the presence of CH3COOH as a catalyst and EtOH as solvent to afford the corresponding target products 6a-e in high yields and purities. The characterization data obtained from elemental analysis, FT-IR, NMR (1H- and 13C-) were in full agreement with the expected structures. Furthermore, an X-ray single crystal diffraction study of one of the target s-triazine hydrazone derivatives, 6c confirmed the structure of the desired compounds. It crystallized in the triclinic crystal system and…
Isostructural Inorganic–Organic Piperazine-1,4-diium Chlorido- and Bromidoantimonate(III) Monohydrates: Octahedral Distortions and Hydrogen Bonds
2020
Halogenidoantimonate(III) monohydrates of the (C4H12N2)[SbX5]·
Synthesis, X-ray structure, Hirshfeld analysis, and DFT studies of a new Pd(II) complex with an anionic s-triazine NNO donor ligand
2020
A new Pd(II) complex, [Pd(Triaz)Cl], with the hydrazono-s-triazine ligand, 2,4-di-tert-butyl-6-((2-(4-morpholino-6-(phenylamino)-1,3,5-triazin-2-yl)hydrazono)methyl)phenol, was synthesized by the reaction of PdCl2 with the organic ligand (1:1) in acetone under isothermal conditions. The molecular structure of the [Pd(Triaz)Cl] complex was determined using FTIR and 1H NMR spectroscopic techniques, and single-crystal X-ray diffraction. Moreover, using Hirshfeld surface analysis, the percentages of the intermolecular interactions were determined. The obtained values were 60.6%, 11.6%, 8.1%, 3.6%, and 5.0% for the H⋯H, C⋯H, O⋯H, N⋯H, and Cl⋯H interactions, respectively. Among them, the O⋯H, C⋯H…
X-ray Crystal Structure and Hirshfeld Analysis of Gem-Aminals-Based Morpholine, Pyrrolidine, and Piperidine Moieties
2020
The gem-aminals of 1,2-dimorpholinoethane (1) and 1-morpholino-3-morpholinium bromide propane (2) were synthesized by reaction of two molar ratio of morpholine with the halogenating agents in the presence of basic condition (K2CO3) in acetone at room temperature (RT) overnight. The structures of the centro-symmetric compound 1 and the morpholinium salt derivative 2 were assigned unambiguous by single crystal X-ray diffraction analysis and compared with the 1,2-di(pyrrolidin-1-yl)ethane 3 and 1,2-di(piperidin-1-yl)ethane 4. The 1,2-dimorpholinoethane molecule has a center of symmetry at the midpoint of the C-C bond of the ethyl moiety leading to two equivalent halves. It crystallized in mono…
Synthesis of C2-Symmetrical Bis-(β-Enamino-Pyran-2,4-dione) Derivative Linked via 1,6-Hexylene Spacer: X-ray Crystal Structures, Hishfeld Studies and…
2021
The synthesis of C2-symmetrical bis(β-enamino-pyran-2,4-dione) derivative 3 connected via 1,6-hexylene linker was reported for the first time. X-ray structures and Hirshfeld studies of the new bis- β-enamino-pyran-2,4-dione derivative 3 along with two structurally related pyran-2,4-dione derivatives 2a,b were discussed. A comparative analysis of the different intermolecular contacts affecting the crystal stability was presented. Generally, the H…H, O…H, and H…C interactions are common in all compounds and are considered the most abundant contacts. In addition, DFT calculations were used to compute the electronic properties as well as the 1H and 13C NMR spectra of the studied systems. All co…
Synthesis and electronic aspects of tetrahydrobenzothienopyrimidine derivatives
2015
Abstract The chemistry of thiophenes, pyrimidines, triazolopyrimidines and benzothiophenes has drawn much attention because of their biological activities. Their interesting properties are connected with their complex π-electron delocalisation effects. Herein the synthesis, crystal and molecular structures at 100 K and DFT calculated structures of three tetrahydrobenzothienopyrimidine derivatives are reported i.e. 4-hydrazino-5,6,7,8-tetrahydro[1]benzothieno[2,3-d]pyrimidine which was a substrate for 2-phenyl-8,9,10,11-tetrahydro[1]benzothieno[3,2-e][1,2,4]triazolo[1,5-c]pyrimidine and 3-methyl-9,10,11,12-tetrahydro-2H-[1]benzothieno[2′,3′:4,5]pyrimido[1,6-b][1,2,4]triazin-2-one. Moreover t…