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ABSTRACT A copper‐based one‐dimensional framework compound [Cu2(L1)4(L2)]n (1) [L1 = 3‐(2‐thienyl)acrylic acid, L2 = 4,4′‐bipyridine] has been synthesized by slow diffusion of layers technique and characterized by spectroscopic methods and single‐crystal X‐ray crystallography. X‐ray diffraction analysis reveals that the compound is crystallized in the triclinic crystal system with space group Pī. Two neighboring Cu centers are bridged by four carboxylato groups from four different L1 ligands, leading to the formation of a paddle‐wheel [Cu2(COO−)4] secondary building unit (SBU). The paddle‐wheel units are interconnected by bidentate 4,4′‐bipyridine ligands to form a one‐dimensional infinite chain network. In [Cu2(L1)4(L2)]n (1), Cu(II) ion features a penta‐coordinated environment around it. Notably, [Cu2(L1)4(L2)]n (1) is capable of activating molecular oxygen to efficiently catalyze the oxidation of alcohols under base‐free conditions. [ABSTRACT FROM AUTHOR]

The synthesis of a novel complex [Ni3 (L3 -)2 (1,4-bib)4 (H2 O)2]·5H2 O (1) with three-dimensional framework structure was achieved through a hydrothermal reaction, employing 5-((4-carboxylphenoxy)-methyl) isophthalic acid (H3 L) as the main oxygen-containing ligand, complemented by the N-donor ligand 1,4-bis(1H-imidazol-1-yl)benzene (1,4-bib), and Ni(II) ions. The structure of complex 1 was characterized by single crystal X-ray diffraction, powder X-ray diffraction, and elemental analysis. Complex 1 is crystallized in the triclinic crystal system of P-1 space group, and its crystallographic parameters are a =1. 260 5(7) nm, b = 1. 349 1(7) nm, c = 1. 364 8(7) nm, α = 111. 913(8)°, β = 117. 251(7)°, γ =90. 732(8)°, V =1. 866 2(18) nm3, Z =1, Mr =1 769. 66, F(000) =916, μ = 0. 84 mm-1, Dc = 1. 575 mg·m-3, S =1. 06, R1 =0. 056, wR2 =0. 159. The joint contribution of semi-rigid tricarboxylic acid ligand L3 -, rigid 1,4-bib and also with Ni(II) ion to form a predictable high-dimensional structure. Complex 1 is a three-dimensional network constructed through the coordination of N and O atoms with Ni ion and the structural extension of the ligand. In addition, the magnetic properties of Ni(II) compound containing single d electron center were studied: the carboxyl group in mononuclear complex 1 only binds to one cation, resulting in magnetism in the solid being determined by the behavior of single metal ions. Variable temperature magnetic susceptibility of　χmT in complex 1 can be described by zero field splitting. [ABSTRACT FROM AUTHOR]

A case of binuclear manganese complex [Mn2 (L)4 (phen)2 (H2 O)2] (1) was synthesized under solvothermal conditions with 2-naphthalic acid (HL) and 1,10-phenanthrenoline (phen) as ligands and manganese carbonate as the metal source. Complex 1 was characterized by single-crystal X-ray diffraction, elemental analysis, fourier transform infrared spectroscopy, powder X-ray diffraction, and thermogravimetric analysis. single-crystal X-ray diffraction shows that complex 1 belonged to the triclinic crystal system P1 space group and the crystal cell parameters are a = 0. 769 89(5) nm, b =1. 175 86(5) nm, c =1. 668 30(9) nm, and α = 107. 074(5)°,β = 96. 167(5)°,γ = 106. 901(5)°. The asymmetric unit consists of a manganese ion, two 2-naphthoate anions, one 1,10-phenanthroline ligand and one water molecule, and Mn(II) atom is in a distorted octahedral configuration. The asymmetric units are bridged by carboxyl-oxygen atoms to form a dinuclear structure and then the binuclear structures are linked into a 2D supramolecular structure through π...π stacking interactions. The results of fluorescence spectroscopy show that complex 1 has good fluorescence performance and the maximum emission wavelength is 416 nm (λex =302 nm). Thermogravimetric analysis shows that complex 1 remains stable to 117 ℃, and then begins to lose water of 3. 18%, the structure after dehydration can stabilize at 223 ℃, after which the organic framework begins to collapse. Hirshfeld surface analysis is used to study the interaction between molecules. [ABSTRACT FROM AUTHOR]

Four alkaline earth metal-based compounds were synthesized under hydrothermal conditions, using BPTC (benzophenone-3,3′,4,4′-tetracarboxylate) as ligand, and are hereinafter referred to as M-BPTC (M = Mg, Ca, Sr, Ba). These compounds exhibit interesting structural diversity, variable chemical and thermal stability, as well as antimicrobial activity and proton conductivity. The Ca-BPTC (C17H13O12Ca) belongs to the triclinic crystal system, P-1 space group (a = 6.9330 Å, b = 9.8359 Å, c = 14.8717 Å, α = 78.351°, β = 81.043°, γ = 71.696°). The Sr-BPTC (C17H10O11Sr2) crystallized into an orthorhombic crystal system, Pbca space group (a = 6.9945 Å, b = 10.3767 Å, c = 47.882 Å and α = β = γ = 90°) and showed proton conduction up to 55 °C. The compound Ba-BPTC (C17H8O10Ba2) belongs to the triclinic crystal system, P-1 space group (a = 4.39030 Å, b = 11.9969 Å, c = 16.0108 Å, α = 71.6830°, β = 86.2360°, γ = 89.790°). The crystal structure of the compound of Mg2+ with BPTC was not elucidated. The calcium coordination polymer and magnesium compound showed antibacterial activity against Staphylococcus aureus and Pseudomonas aeruginosa and antifungal activity against Candida albicans. [ABSTRACT FROM AUTHOR]

In this present investigation, a new series of functionalized hybrid compounds containing three bioactive triheterocyclic templates, pyrazolines, thiazolidinones, and indolones are designed and synthesized via multicomponent, one-pot reaction of 3-(4-chlorophenyl)-5-[4-(propan-2-yl)phenyl]-4,5-dihydro-1H-pyrazole-1-carbothioamide with various substituted isatin derivatives and chloroacetic acid in the presence of fused sodium acetate and glacial acetic acid viz ring closure mechanism followed by dehydration. The formation of new scaffolds 4–7(a–c) is evidenced by analytical and spectral studies. The single-crystal X-ray diffraction study supported the molecular structure of compound 4a as a triclinic crystal system with a P 1 ¯ space group and Z = 2. Interestingly, the compound is crystallized with two molecules (A/B) and one water molecule in the asymmetric unit, and the crystal packing is stabilized by intra and intermolecular hydrogen bonds. To quantify the percentage of intermolecular contacts and electrostatic potential distribution in crystal packing, Hirshfeld surface analysis was performed. All the compounds were screened for their preliminary antimicrobial activity against a panel of bacterial and fungal strains. The newly synthesized compounds exhibited fairly encouraging in vitro antibacterial activity, so the validation of the potent compound was done by docking against the antibacterial target Escherichia coli FabH (PDB: 5BNS). The virtual screening is focused on ADME and drug-likeliness properties to identify their putative ligand-protein interactions using Schrödinger software. [ABSTRACT FROM AUTHOR]

Novel nickel(II) ethylenediamine compound, [Ni(en)3](2-chlorophenylacetate)2, has been synthesized and characterized by spectroscopic techniques (UV-vis, FT-IR), thermogravimetric analysis, magnetic moment, molar conductivity measurement, and single-crystal X-ray diffraction analysis. The complex crystallizes in a triclinic crystal system with P 1 ¯ space group with cell dimensions of a = 8.9050(2), b = 12.5620(4), c = 14.0590(4) Å, α = 102.259(2)°, β = 107.172(2)°, and γ = 106.914(2)°. The complex consists of [Ni(en)3]2+ as the cationic part and two discrete 2-chlorophenylacetate ions as anionic counterparts divulging the existence of a second sphere complex with distorted octahedral geometry. Besides electrostatic forces of attraction, non-covalent interactions (hydrogen bonding and C-H...π) sew the second sphere in extended three-dimensional supramolecular architecture and provide robustness to the crystal lattice. Field electron scanning microscope (FESEM) and energy dispersive X-ray spectra (EDX) were employed to study the surface morphology of the structure. To explore the structural insights and bonding in the complex theoretical studies, i.e., density functional theory (DFT) and Hirshfeld surface analysis have also been employed. [ABSTRACT FROM AUTHOR]

A novel hydrogen bonded single crystal of 7-azaindolinium-3,5-dinitrobenzoate (7AIDNB) has been grown, and the structure of the crystal was determined by single-crystal XRD analysis. The results show that the grown crystal belongs to a triclinic crystal system with centrosymmetric space group P-1 and the unit cell parameters: a = 6.998(9) Å, b = 8.498(12) Å, c = 13.103(17) Å, V = 710.78(17) Å3, Z = 2. The presence of expected discrete functional groups in 7AIDNB has been identified by an FT-IR spectroscopic study. The thermal stability and decomposition of the title crystal have been studied by TG-DTA analysis. The optical property of the grown crystal has been analyzed by UV-Vis-NIR spectroscopy analysis. The DFT with 6-311++G(d, p) basis set has been used to examine optimization of molecular geometry, Mulliken charge, and HOMO-LUMO. As the frequency of the grown crystal increases, the dielectric loss and dielectric constant decrease. The third-order NLO parameters of 7AIDNB have been examined by a Z-scan technique. [ABSTRACT FROM AUTHOR]

Sr 2 V 2 O 7 (SVO) microwave dielectric ceramics were fabricated through a conventional solid-state synthesis method and sintered at 900–1000 °C for 10 h. The crystal structures and morphologies of the SVO samples were examined via X-ray diffraction and scanning electron microscopy. These analyses revealed that the SVO sample sintered at 950 °C exhibited high crystallinity and a triclinic crystal system. Through the lens of lattice dynamics, the phonon characteristics of the SVO samples were investigated via Raman spectroscopy and far-infrared spectroscopy to elucidate the dielectric response mechanics and microstructural origins of these responses. Raman spectra were classified into three sections corresponding to the vibration of Sr2+ ions, the V–O or V–O–V telescopic vibration, and the internal elongation of the tetrahedral structure composed of V–O, respectively. The inherent dielectric properties obtained from the far-infrared spectra were analyzed using a four-parameter semi-quantum model with the assistance of the Focus software. This analysis aligned with the measured property values. The relationships between the crystal structures and the dielectric properties were established using the Raman modes. Particularly, the SVO sample sintered at 950 °C exhibited excellent dielectric properties, characterized by a dielectric constant (ε r) of 9.49, a quality factor (Q × f) of 35,189 GHz, and a resonant frequency (f) of 12.48 GHz. [ABSTRACT FROM AUTHOR]

The successful growth of 2-Methylbenzimidazolium 4-nitrobenzoate 4-nitrobenzoic acid (MINB) from a solution of ethyl and methyl alcohol using the solvent evaporation solution technique (SEST). The MINB crystal belongs to the triclinic crystal system and possesses a centrosymmetric P-1 space group, maintained by N–H...O and O–H...O interactions. Proton configuration confirmation was achieved through 1H-NMR analysis, while FTIR and Raman studies identified functional groups and vibrational frequencies. Optical transmission analysis revealed exceptional transparency (> 90%), along with a cut-off wavelength at 400 nm and Eg = 2.91 eV. The crystal's thermal behaviour was studied using thermogravimetric and differential thermal analysis, etching studies assessed crystal perfection, Vicker's microhardness test determined load-dependent hardness, and dielectric properties (ε′, δ) were measured at 313 K with the frequency range of 50 Hz to 5 MHz. Nonlinear optical characteristics were explored using Q-switched Nd:YAG laser with a wavelength of 532 nm, exhibits Reverse saturable absorption (RSA) has been triggered by Two-Photon Absorption (2PA). The nonlinear absorption coefficient (β) of MINB crystal increased with concentration of solution, while the optical limiting threshold decreased with higher MINB concentrations, showcasing its intriguing properties and potential applications. We exploited First-principles density functional theory and ab-initio molecular dynamics simulations to investigate the electrical and optical characteristics of the MINB material. We establish that this material exhibits semiconductor properties, characterized by an energy band gap of 2.86 eV and notable absorption in the Ultraviolet (UV) light spectrum. [ABSTRACT FROM AUTHOR]

The first rare-earth borate crystal CsBa2 ScB8 O16 with both zero-dimensional [B3 O6] units and one-dimensional B--O chain structures has been synthesized by the high-temperature solution method. It crystallizes in the triclinic crystal system with the P1 space group, with lattice parameters of a =6.698 5 Å, b =7.216 Å, c =14.798 Å, α =97.563°, β =95.226°, γ = 95. 546°, Z = 2. In this compound, [BO3] and [B4 O9] units are connected by sharing oxygen atoms to form a onedimensional chain [B5 O10]∞. Octahedrally coordinated [Sc(1)O6] groups and the one-dimensional chain [B5 O10]∞ are further connected by sharing oxygen atoms to form two-dimensional layer [Sc(1) (B4 O9)]∞. Interlayers are linked by octahedrally coordinated [Sc(2)O6] groups, which share oxygen atoms to form a three-dimensional Sc--B--O framework. Isolated [B3 O6] units are filled in the three-dimensional channels with Cs+ and Ba2 + to balance the charges. In order to further explore the novelty of the structure of CsBa2 ScB8 O16, we compared it with other rare-earth borates containing alkali or alkaline-earth metals, and discuss the effect of the cation-to-boron molar ratio (n(A) / n(B)) on the degree of polymerization of B--O units, as well as the dimensionality of the B--O anion framework. Furthermore, the first-principles calculations, infrared spectrum, UV-vis-NIR diffuse reflectance spectrum and the thermal analysis of the compounds have also been performed. Property measurements show that CsBa2 ScB8 O16 exhibits short UV absorption edge (< 190 nm) and moderate birefringence (0. 072@1 064 nm). The optical properties of the compound are mainly contributed by the [B3 O6], [B5 O10] units, and [ScO6] octahedra. [ABSTRACT FROM AUTHOR]

Features of the crystallization of various compounds on the Nafion polymer substrate from supersaturated aqueous solutions is studied by XRD. The solutions are prepared from natural deionized and deuterium-depleted water. It was earlier established that the swelling of Nafion in natural deionized water clearly demonstrates effects caused by the partial uncoiling of polymer fibers into the liquid volume, but no such effects were observed in deuterium-depleted water. The ab initio calculations performed in the present work show that the uncoiling of lateral Nafion chains with terminal –SO3H groups and the dissociation of these groups with subsequent formation of hydronium ions and structural anionic residues are energetically favorable in the case of the contact with a sufficient amount of water molecules. The influence of these factors on the process of crystal formation on polymer substrates is studied. It is established that the effect of partial uncoiling of polymer chains indeed affects the crystallization, and does it in different ways, depending on the crystal structure. Thus, no differences between XRD patterns of crystals grown on smooth and polymer substrates are observed for the monoclinic lattice of sodium acetate trihydrate. In the case of copper sulfate (with either CuSO4·5H2O pentahydrate crystals (triclinic crystal system) or CuSO4·3H2O trihydrate crystals (monoclinic crystal system)), copper sulfate trihydrate and pentahydrate are formed on the polymer and smooth substrates, respectively. None of the studied crystals exhibited differences between smooth and polymer substrates for the supersaturated solutions based on deuterium-depleted water, and in both cases a triclinic crystal system of the CuSO4·5H2O pentahydrate precipitate is identified for the CuSO4 aqueous solution. For sucrose, the precipitate amorphization upon the deposition onto the Nafion plate is detected. A theoretical model is proposed to explain the effect of partial polymer chain uncoiling on the growth of crystals, depending on their crystal system, unit cell parameters, and the volumetric ratio of hydrophilic and hydrophobic fragments in the molecular structure. [ABSTRACT FROM AUTHOR]

The single crystal of the title compound Diethyl 1-(4-nitrobenzyl)-4-(4-nitrophenyl)-2,2-dioxooctahydro-2-pyrrolo[2,1-c]1,4thiazine-1,3-dicarboxylate was grown and characterized by single crystal X-ray diffraction technique. Further, Hirshfeld surface, quantum chemical, and molecular docking analyses of the compound were carried out. The title compound was crystallized in a triclinic crystal system with a centrosymmetric space group of P-1 and has one molecule in the asymmetric unit. The stability of the grown crystal structure was confirmed by the C-H...O and π...π interactions. The hydrogen bonding features were analyzed and the prominent intermolecular interactions present in the structure were investigated using Hirshfeld surface analysis. The interaction energy between pairs of the molecule was obtained from Energy Framework analysis. The molecular structure of the title compound was optimized using density functional theory calculation in the ground state and the calculated structural parameters of the compound were compared with the experimental XRD data. Mulliken atomic charge distribution and frontier molecular orbitals analyses were also carried out to validate the reactivity of the title molecule. Molecular docking studies confirm that the title compound has potent inhibitory nature against the human mutant HIV-1 reverse transcriptase protein. Thus, the present study paves the way for the development of a novel HIV-1 drug. [ABSTRACT FROM AUTHOR]

A novel 2,4-dibromo-6-(1H-phenanthro[9,10-d]imidazol-2-yl)phenol crystal has been reported and characterized by FT-IR, 1H NMR, 13C NMR. Single crystal XRD studies reveals that the compound crystalizes into triclinic crystal system with P-1 space group, and crystallographic data has been deposited in the Cambridge crystallographic data center with CCDC Number: 2246180. Various computational analysis like, Hydrogen bond analysis, Molecular electrostatic potential analysis, Natural population analysis, hirshfeld surface, and Frontier molecular orbital analysis were performed to elucidate the structure of the crystal. Marcus-Hus semiclassical model for charge transfer in organic materials is applied for the calculation of charge transfer rate. The calculation of reorganization energy and coupling constant reveals that the compound could be investigated as hole transport material. Synthesis, characterization, and computational analysis of Imidazole-based Organic crystals as charge transport material. [ABSTRACT FROM AUTHOR]

Reaction of 4,6-dinitroresorcinol (1) and the nitrogen base 1,4-diazabicyclo[2·2·2]octane (2) affords the 1:2 salt and proton-transfer compound 1,4-diazabicyclo[2·2·2]octane-1,4-diium bis(5-hydroxy-2,4-dinitrophenolate) (3). Compound 3 crystallizes in the triclinic crystal system (space group P-1) with a = 8.3242(5) Å, b = 11.9915(7) Å, c = 12.4595(7) Å, α = 116.282(2)°, β = 100.576(3)°, γ = 101.051(2)°, 1042.30(11) Å3 and Z = 2. The dication 2- H 2 2 + forms charge assisted donating bifurcated N+−H⋅⋅⋅O− hydrogen bonds to the phenolate moieties of two monoanions of 1. The latter exhibit an intramolecular O−H⋅⋅⋅O hydrogen bond between the hydroxy group and the nitro group in ortho position. The crystal structure of 3 features pseudo B-centering of the lattice, which relates the two crystallographically distinct monoanions of 1 by a pseudo translation. The possible B-centring is broken by the ethylene groups of 2-H22+, which are related in neighbouring molecules by centres of symmetry. [ABSTRACT FROM AUTHOR]

The preparation and characterization of Cu 1·7 Mo 0·3 O 4 and Cu 1·4 Mo 0·6 O 4 nanostructures using the gelatin/sol-gel combustion method have been reported. The synthesized materials were investigated using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (cSEM), surface area analysis, and optical measurements. UV–Vis absorption spectra of the nanocomposites were analyzed to investigate the absorption and bandgap energy of the optical band gap. The Cu 1·7 Mo 0·3 O 4 nanomaterial show cased a triclinic crystal structure system, while the Cu 1·4 Mo 0·6 O 4 exhibited an orthorhombic system. The BET surface area analysis of the catalysts has values of 53 and 502 m2/g. The Cu 1·7 Mo 0·3 O 4 sample proved to be the most active in generating hydrogen through NaBH 4 methanolysis, displaying an impressive production rate of 23,063 mL/g. min. The findings indicate that the addition of Cu 1·7 Mo 0·3 O 4 improves the catalytic activity of the methanolysis reaction involving sodium borohydride. • Synthesized of Cu 1·7 Mo 0·3 O 4 and Cu 1·4 Mo 0·6 O 4 using the gelatin/sol-gel combustion method. • The average crystalline size was obtained for Cu 1·7 Mo 0·3 O 4 to be 32.7 nm while 60.5 nm for Cu 1·4 Mo 0·6 O 4. • The BET surface area of Cu 1·7 Mo 0·3 O 4 and Cu 1·4 Mo 0·6 O 4 analysis of the catalysts has values of 53 and 502 m2/g. • Cu 1·7 Mo 0·3 O 4 catalyst attains a high generation rate of 9191 mL/g. min. [ABSTRACT FROM AUTHOR]

Kermesite (Sb2S2O), a needle-like unstable secondary oxysulfide, has made visible advancements in optimizing its triclinic crystal system through twinning discovery. However, research on twinning behavior at micro and nano scales, including its growth mechanisms and impact on kermesite morphologies, remains notably scarce. Our study focuses on kermesite crystal clusters from a private collection in Yunnan, China, confirming the chemical formula as Sb2S1.97O1.03 through EPMA. Single-crystal XRD yielded refined unit cell parameters (a = 8.153(5) Å, b = 10.717(7) Å, c = 5.796(3) Å; α = 102.836(10)°, β = 110.556(8)°, γ = 100.999(12)°), revealing space group P 1 ¯ with Z = 4 and indicating twinning with a ratio of 27.4%. Remarkably, a Transmission Electron Microscope (TEM) provided the first direct observation of twinning in natural kermesite, revealing rotational twins with varying widths and lengths (ranging from 100 nm to several millimeters). Analysis and simulation elucidated that rotational twins, generated by a 180° rotation, align with the mineral's elongation direction along the [Sb2S2O4]n chains (a-axis), challenging the conventional long-axis direction (b-axis) for crystal growth. This study proposes a symbiotic relationship between kermesite growth and twinning, suggesting that the observed X-shaped growth in crystal clusters results from the collaboration of single crystals (growing along b) and twins (growing along a) in the unit cell. These findings contribute to our understanding of kermesite's structural complexities and the potential growth and formation mechanism of crystal clusters. [ABSTRACT FROM AUTHOR]

Crystallographic features of the synthesized compound (E)-4-methoxy-2-(((2-methoxy-5-(trifluoromethyl) phenyl)imino)methyl)phenol are investigated with the Hirshfeld surface analysis and X-ray diffraction (XRD). The stability of the crystal packing primarily stems from N–H⋯O and C–H⋯O bonding interactions, further fortified by offset π⋯π stacking interactions. To delve into the supramolecular arrangement, the Hirshfeld surface analysis is conducted, shedding light on the intricacies of the crystal packing. The structure of the synthesized compound is determined through the single crystal XRD analysis, revealing its crystallization within the triclinic crystal system, space group . The supramolecular assembly is explored by the Hirshfeld surface analysis, and the supramolecular geometric features of the title compound involve the compact arrangement of title molecules with each other. The dispersion energy properties are examined through studies on the interaction energy and energy frameworks. [ABSTRACT FROM AUTHOR]

A 0D Cu-based complex (1) (Cu(L)2(EDA)2]n, L = 3-phenylpropylmalonic acid, EDA = ethylenediamine) is synthesized by the solvent-thermal synthesis using 3-phenylpropylmalonic acid as the ligand. It is characterized and analyzed by powder X-ray diffraction, IR and UV diffuse reflectance spectroscopy, and other techniques. Complex 1 crystallizes in the triclinic crystal system with space group , and each Cu2+ is coordinated with two ligands and a water molecule, respectively. The cyclic voltammetry curve of the electrode modified by 1 (1+CPE) is tested in the PBS buffer solution (pH = 6.5). The found pair of reversible redox peaks belonging to Cu(II)/Cu(I) prove that 1 can be used in electrochemical applications. [ABSTRACT FROM AUTHOR]

The development of electrochemical sensors operating at low potentials is a promising method for monitoring environmental toxicants. In this research study, we designed and synthesized a redox active material, ferrocene conjugated biphenyl pyridine acrylonitrile (Fc-BPy), and applied it for the low potential non-enzymatic detection of catechol (CC) through electrochemical technique. Fc-BPy was systematically characterised using single-crystal XRD (SC-XRD). Fc-BPy crystallizes in a triclinic crystal system with a P-1 centrosymmetric space group. The electrochemical investigation of the Fc-BPy/GCE modified electrode exhibits a well-defined redox peak at a low anodic (Epa) and cathodic (Epc) peak potential of 0.32 V and 0.21 V, respectively, which favours the non-interference and selective detection of CC. Furthermore, commendable conductivity was achieved in the absence of any other conducting material due to a profound charge transfer between Fc-BPy and the electrode surface. In amperometry, Fc-BPy/GCE shows excellent non-enzymatic electrocatalytic activity towards CC over a linear detection range from 20 μM to 1.02 mM. The sensitivity and limit of detection (LOD) of CC were found to be 36.42 mM μA−1 cm−2 and 6.2 μM, respectively. Additionally, the fabricated sensor showed consistent performance over multiple cycles and extended periods of storage. The practical utility of the sensor for the detection of CC was tested in various real-time samples. The results were astounding with good recovery rates. Thus, the fabricated sensor exhibits a striking performance for the non-enzymatic detection of CC at a low potential with a high sensitivity, selectivity, better linear range, and low limit of detection. [ABSTRACT FROM AUTHOR]

The reaction of 5-cyano-1,2,4-triazines with 5-(methylsulfanyl)-4H-1,2,4-triazol-3-amine under solvent-free conditions gave product of nucleophilic substitution of the cyano group of 1,2,4-triazine by the 1,2,4-triazol-3-amine residue. The product structure was determined by 1H NMR and mass spectrometry (electron impact). Its 1H NMR spectrum showed a characteristic three-proton singlet at δ 2.61 ppm, which was assigned to methylsulfanyl group. The subsequent reaction of the obtained product with norborna-diene under pressure resulted in the transformation of the 1,2,4-triazine ring into pyridine, while the methyl-sulfanyl group remained intact. This was confirmed by X-ray analysis of the resulting functionalized pyridine. According to the X-ray diffraction data, it crystallized as two crystallographically independent molecules in non-centrosymmetric space group P-1 belonging to the triclinic crystal system. The crystal structure is formed via numerous intermolecular N···H contacts between the two crystallographically independent triazolylpyridin-2-amine molecules. The 1H NMR spectrum displayed two doublets at δ 7.37 and 7.61 ppm due to protons of the newly formed pyridine ring. Thus, the behavior of 5-(methylsulfanyl)-4H-1,2,4-triazol-3-amine differs from the behavior of its analogue containing a thiol group at C5. As we showed previously, in the reaction of the latter with 5-cyano-1,2,4-triazine, substitution of the cyano group was accompanied by desulfurization of the triazole-5-thiol. [ABSTRACT FROM AUTHOR]

The synthesis and crystal structure of 2-bromo-4,6-bis(dibromoacetyl)resorcinol, I, was reported. In the title compound, I, crystalized in the triclinic crystal system with Pī space group. The two carbon and the oxygen atom of the acetyl groups (atoms C7, C8, O3, and C9, C10, O4) are nearly co-planar with the central phenyl ring. Intramolecular O–H···O, C–H···Br, and intermolecular C–H···Br/O interactions, two non-bonded contacts (Br5···Br3 and O4···C8) and π-π stacking interaction are stabilized the crystal packing of the title compound. Intermolecular interactions that exist in the title compound, I, are quantified with the aid of PIXEL and Hirshfeld surface (HS) analysis and the decomposed fingerprint (FP) plots. The FP plot reveals that the Br···Br contacts are comparably higher than the other contacts in the title crystal structure. Furthermore, the theoretical density functional theory (DFT) calculations were performed at the M062X/cc-PVTZ level of theory. The experimental geometry parameters of the title molecule are compared with the geometry of the optimized molecule in the gas phase. The chemical reactivity and charge transfer properties of the title compound were calculated from the HOMO and LUMO energy. In addition, the molecular electrostatic potential map was generated at their crystal structure geometry and quantitatively analyzed. [ABSTRACT FROM AUTHOR]

The invention discloses a preparation method for nickel (II) nitrate hexahydrate boric acid and the growth of single crystals by the slow evaporation solution growth technique. Single crystal x-ray diffraction (XRD) analysis shows N2NHB crystallize in triclinic P crystal system with lattice parameters of a = 6.61 Å, b = 7.05 Å, c = 7.07 Å, α = 119.61°, β = 92.25°, γ = 101.11° and volume = 278 Å3. The chemical composition and the corresponding functional groups of the grown crystal have been identified by EDAX and FTIR analyses. Scanning electron microscope (SEM) pictograph indicated that the particles were closely spherical in shape with slight agglomeration. UV–Visible studies shows N2NHB crystal exhibit lower cut-off wavelength of 314 nm, wide optical window (320 – 800 nm) and wide band gap of 4.16 eV. According to the fluorescence spectrum, the emission occurs at a wavelength of 533 nm. Different temperatures were used to study the Grown crystalc dielectric behaviour. A positive photocurrent is found in the Grown crystal, as shown by the photoconductivity analysis. The second harmonic generation (SHG) capability was demonstrated by the standard Kurtz and Perry powder method. Open aperture Z-scan technique reveals that the material exhibits two-photon absorption phenomenon with nonlinear absorption coefficient of 0.75 × 10−11 m/W. The material displays optical limiting behaviour with an onset limiting threshold of 4.72 × 1012 W/m2. Altogether the grown N2NHB crystal can be utilized wide variety of optoelectronic applications of which optical limiting activity for laser safety devices is notable. [ABSTRACT FROM AUTHOR]

The title compound, (C4H12N)[V(C12H8N4O2)O2]H2O, was synthesized via aerial oxidation on refluxing picolinohydrazide with ethyl picolinate followed by addition of VIVO(acac)2 and diethylamine in methanol. It crystallizes in the triclinic crystal system in space group P.... In the complex anion, the dioxido-vanadium(V) moiety exhibits a distorted square-pyramidal geometry. In the crystal, extensive hydrogen bonding links the water molecule to two complex anions and one diethylammonium ion. One of the CH2 groups in the diethyl-amine is disordered over two sets of sites in a 0.7:0.3 ratio. [ABSTRACT FROM AUTHOR]

A cluster complex of the composition [{Re6Te8}(TeI2)6]I2·[{Re6Te8}(TeI2)4(TeI3)2]·I2 is obtained by a reaction between [{Re6Te8}Te7] and I2 in a sealed quartz ampoule at 400 °C. More than three times increase in the volume of the ampoule in which the reaction is performed with maintaining the other conditions is shown to lead to the formation of the previously described cluster complex [{Re6Te8}(TeI2)6]I2. An increase in the synthesis temperature to 450 °C leads to the formation of X-ray amorphous products of the unknown composition. The [{Re6Te8}(TeI2)6]I2·[{Re6Te8}(TeI2)4(TeI3)2]·I2 compound obtained at 400 °C crystallizes in the triclinic crystal system, space group , and unit cell parameters a = 11.0859(3) Å, b = 11.9021(4) Å, c = 21.1308(7) Å, α = 79.259(2)°, β = 85.533(2)°, γ = 66.220(2)°, V = 2506.55(14) Å3, Z = 1. The crystal structure consists of four layers of two types that alternate along the c parameter: 1) the layer formed by iodine anions and [{Re6Te8}(TeI2)6]2+ cluster cations and 2) the layer formed by neutral cluster complexes [{Re6Te8}(TeI2)4(TeI3)2] and crystallization I2 molecules. Weak interactions between the adjacent cluster complexes are observed in both layers along with I⋯I halogen bonds. The layers are linked with each other via I⋯I and Te⋯I interactions. [ABSTRACT FROM AUTHOR]

This paper reports the crystal structures of two n-tetrabutylammonium inclusion compounds of 2,2'-bis(4-hydroxyphenyl)propane (BPA) of (n-C4H9)4N+⋅C15H15O ⋅3C15H16O2⋅C2H5OH (1) and 2(n-C4H9)4N+⋅C2O ⋅2C15H16O2 (2), which were characterized by single crystal X-ray diffraction. The experimental data show that 1 can be classified to be the triclinic crystal system of P space group and 2 to be the orthorhombic system of Pna21 with higher symmetry. Interestingly, the crystal structures of the two inclusion compounds have the same point during the formation of the related structures. In these two crystals with varied symmetry, BPA molecules or ions and the bridging auxiliary molecules first form a separate hydrogen bond unit, then the hydrogen-bonded units pack to form the three-dimensional host framework by different symmetry operations. And finally the guest tetrabutylammonium cations are arranged between the varied voids of the host skeleton to yield the stable crystalline structures. [ABSTRACT FROM AUTHOR]

We employed a dual strategy that combines experimental and computational analyses of two copper(II) coordination complexes with σ-donating acylpyrazolone ligands. HLIIIB, [Cu(HLIIIB)2] and [Cu(HLI)2] have been characterized using a variety of physicochemical methods and density functional theory (DFT) calculations using the B3LYP level of theory and 6-31 G basis set. Single crystal X-ray diffraction studies revealed monoclinic and triclinic crystal systems for [Cu(HLI)2] and [Cu(HLIIIB)2], respectively, with square planar geometries for both complexes. Both complexes exhibit quasi-reversible behavior in their cyclic voltammograms in DMSO. ESR spectroscopy was performed to determine the magnetic behaviorof the two complexes. The intermolecular interactions of the complexes were further investigated using Hirshfeld surface analysis. The compounds showed promising cytotoxicities when tested against cancer cell lines of lung carcinoma, hepatocellular carcinoma, and neuroblastoma. Notable apoptotic cell death was observed with [Cu(HLI)2], supported by gene expression changes, indicating induction of apoptosis. The findings suggest the potential of copper complexes as effective agents against neuroblastoma and highlight their superiority to cisplatin. [ABSTRACT FROM AUTHOR]

Selenaphosphocine [(–OC6H2(tBu)2(µ-Se)(tBu)2C6H2O–)PhP] (1) on treatment with [Pd(COD)Cl2] yielded P,Se-coordinated complex [{(–OC6H2(tBu)2(µ-Se)(tBu)2C6H2O–)PhP}(PdCl2)] (2), whereas the reaction of 1 with [AuCl⋅SMe2] resulted in only P-coordinated complex [{(–OC6H2(tBu)2(µ-Se)(tBu)2C6H2O–)PhP}(AuCl)] (4). The reaction of 1 with [Rh(CO)2Cl]2 in 4:1 molar ratio yielded a rare RhIII octahedral complex [{PhP(–OC6H2(tBu)2(µ-Se)(tBu)2C6H2O–)}{PPh(–OC6H2(tBu)2)(Se(tBu)2C6H2O–)}(RhCl)] (3) in good yield, in which one of the C–Se bonds of selenophosphocine is added oxidatively to RhI. All of the complexes have been structurally characterized and are crystallized in the triclinic crystal system with P¯1 space group. All complexes showed intermolecular C–H⋯O and C–H ⋯Se hydrogen bonding interactions, that play major role in the crystal packing to form a three-dimensional array. In complex 2, the crystal packing reveals the presence of rare intermolecular Pd⋯Cl interactions. Hirshfeld surface analysis, dnorm and two-dimensional fingerprint plots were investigated to validate the contributions of the different intermolecular contacts within the supramolecular structure. A Hirshfeld surface analysis indicated that the most significant contributions to the crystal packing of 2 are from H⋯H (66.3%), C⋯H/H⋯C (13.5%), Cl⋯H/H⋯Cl (13.7%), Cl⋯C/C⋯Cl (1.8%) and Cl⋯C/C⋯Cl (1.0%) contacts, and those for 3 are from H⋯H (88.3%), C⋯H/H⋯C (8.3%) and Se⋯H/H⋯Se (3.6%) contacts, while those for 4 are from H⋯H (71.5%), C⋯H/H⋯C (9.9%), Cl⋯H/H⋯Cl (10.2%), Se⋯H/H⋯Se (2.7%) and Au⋯H/H⋯Au (1.7%) contacts. This paper describes the cleavage of a C–Se from dioxaselenaphosphocine and its oxidative addition to rhodium(I) complex and Hirshfeld analysis. [ABSTRACT FROM AUTHOR]

By means of single-crystal X-ray diffraction analysis, vibrational, optical, photoluminescence, and thermal examination, a novel crystal of 2-amino-3-picolinium arsenate has been produced and described. The developed crystal crystallized in triclinic crystal system with centrosymmetric space group P-1 was confirmed by single-crystal XRD investigation. The lattice parameters are calculated as follows: a = 7.28 Å, b = 8.15 Å, c = 8.46 Å, α = 76.98°, β = 79.27°, γ = 88.30°, and volume of the unit cell V = 480.51 (Å)3. The 2-amino 3-picolinum cations and arsenate anions are present in the molecular structure, according to the FT-IR and FT-Raman spectrum studies. The hydrogen and carbon molecular environment are present in the chemical, according to the proton and carbon NMR spectrum. UV–Vis spectral and photoluminescence analysis have been performed to study optical characteristics of the grown crystal. DSC analysis was used to measure heat flow as a function of temperature. Crystal explorer software was used to calculate the Hirshfeld surface, and the 2D finger plot provides insight into the overall packing characteristics of the developed molecule. [ABSTRACT FROM AUTHOR]

In this paper, two novel Cu(II) complexes [CuL(S‐1‐amino‐2‐propanol)] (R1) and [CuL(S‐2‐amino‐1‐propanol)] (R2) have been synthesized and characterized using Fourier transform infrared (FT‐IR), thermogravimetric analysis (TGA), high‐resolution mass spectrometry (HR‐MS), scanning electron microscopy (SEM) and single crystal X‐ray diffraction (SCXRD) technique. The single‐crystal XRD analyses show that compounds R1 and R2 crystallized in triclinic and monoclinic crystal systems with P‐1 and P21 space groups, respectively. The τ5 parameter values of R1 and R2 confirmed distorted square pyramidal geometry around Cu(II) centre. The compounds R1 and R2 possess 2D polymeric chains with (4,4)IIIa and 2C1 topology, respectively. The non‐covalent interactions and electrostatic properties were investigated using Hirshfeld surface analysis and density functional theory (DFT). DFT calculations revealed higher stability of R1 over R2. The presence of strong hyper conjugative interactions in carbon–carbon and carbon–nitrogen bonds has been confirmed by natural bond orbital (NBO) analysis. Time‐dependent (TD)‐DFT calculations were also performed to determine the excited state properties. Based on theoretical calculations, the simulated spectra showed absorption maxima at 506 and 743 nm for both complexes. Antimicrobial assays revealed that R1 is significantly antimicrobial against Pseudomonas aeruginosa at 512 and 256 μg/mL for Staphylococcus aureus, correspondingly. Serum binding studies of R1 confirm the existence of instinctive bonding interactions due to negative values on account of ∆G, ∆S and ∆H obtained from thermodynamics studies. In silico molecular dynamics and docking approaches have been used to validate the experimental findings of anti‐microbial assay and serum binding studies. A high dock score for R1 over R2 revealed the high binding energy of the former with bacterial protein. It was found that the protein‐ligand complex remained stable throughout the dynamic simulation process, and substantial interactions between R1 and bovine serum albumin were observed. [ABSTRACT FROM AUTHOR]

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, where a = 6.23510(10) Å, b = 26.0156(4) Å, c = 12.4864(2) Å, β = 93.243(2)° and the space group is P21. The triazole and indole rings are found twisted from each other in both compounds. The twist angle is higher in 3 (12.65°) than 1 (4.94–7.22°). In the case of the former, the H...H (39.6%), H...C (22.0%), N...H (12.8%) and Br...H (13.2%) contacts are the most dominant while the C...C, C...H, Br...H, N...H and S...S contacts have the characteristics of strong interactions. In the latter, the C...H, N...H, S...H, S...S, and C...C contacts are the most important. In this case, the percentages of the H...H, C...H, N...H and S...H contacts are in the range of 34.9–37.4, 20.5–24.0, 12.2–13.6, 14.0–15.8, respectively. In both systems, the shape index and curvedness of surfaces confirmed the presence of π–π stacking interactions. [ABSTRACT FROM AUTHOR]

An unsymmetrical Schiff base 2-(1-(2-aminophenylimino)ethyl)phenol (LH3) and its trinuclear Pd(II) complex [PdII3(LH)3] (1) were successfully synthesized and X-ray crystallographically characterized. 1 effectively catalyzed Suzuki-Miyaura coupling on reaction between each of bromobenzene and substituted bromobenzenes with phenylboronic acid resulting biphenyl and substituted biphenyls, respectively. The catalyzed products were characterized gas chromatographically. An unsymmetrical Schiff base 2-(1-(2-aminophenylimino)ethyl)phenol (LH3) and its trinuclear Pd(II) complex [PdII3(LH)3] (1) were synthesized, and characterized both spectroscopically and X-ray crystallographically. LH3 and 1 were found to had Cc and P-1 space groups with monoclinic and triclinic crystal systems. 1 was found to catalyze Suzuki-Miyaura cross coupling reactions to produce biphenyl and p-nitrobipheenyl from respective bromobenzene and p-nitrobromobenzene. [ABSTRACT FROM AUTHOR]

We present complementary investigations of water and anion dynamics in an ionic [Cu(H2O)4](ReO4)2. This compound has one reversible phase transition in the solid state upon heating and cooling at 247 and 224 K, respectively. The value of entropy change indicates a moderate degree of molecular dynamical disorder. At room temperature, tetraaquacopper(II) rhenate(VII) crystallizes in a triclinic crystal system, within the space group No. 2 = P‐1, with one molecule in the unit cell. X‐ray single crystal diffraction measurements indicate that the crystal structure does not change significantly at the phase transition. However, neutron diffraction experiments performed on the powdered sample revealed some subtle changes in the registered patterns. Vibrational–reorientational dynamics of H2O ligands in the high (I) and low‐temperature (II) phases of [Cu(H2O)4](ReO4)2 was probed by a set of complementary spectroscopy techniques in a wide temperature range. The dynamics of the H2O molecules in both phases was investigated by means of band shape analysis performed for infrared bands. The H2O ligands perform fast (τR ≈ 10−11 to 10−12 s) stochastic reorientational motions in the phases I and II with a mean value of activation energy: 6.13 kJ⋅mol−1. However, a continuous change of bands connected with hydrogen bonds is observed. The Raman measurements revealed that in the phase transition region the intensity of bands connected with perrhenate anion significantly increases. Using vibrational spectroscopy methods all characteristic wavenumbers of the H2O and ReO4− vibrations were detected. [ABSTRACT FROM AUTHOR]

In synthetic fabrication, the process parameters decide the growth nucleation, phase translation, and the evolution of morphological facets of nanostructured materials. This work demonstrates the formation of different crystallographic phases of calcium phosphate by the influence of pH from acidic to alkaline conditions and also investigated their bone regeneration, protein adsorption, and pro‐angiogenic properties. Present results illustrate that the alteration of pH is the crucial factor for the synthesis of calcium phosphate (CP) phases. The structural analysis reveals the monetite (CaHPO4) phase with a triclinic crystal system for pH 5, dual‐phase of monetite combined with hydroxyapatite at the neutral pH 7, and pure phase of hydroxyapatite (Ca10[PO4]6OH2) with hexagonal structure at pH 10. Microscopic analysis portrays the cubic and rod‐like morphologies by changing the pH values. FTIR and RAMAN spectroscopic analyses confirm the stretching, bending, and vibrational modes of dominant phosphate groups of different CP phases. Further, the biocompatibility of the prepared CP phases was examined by hemolysis assay, which showed less than 2% of lysis and enhanced cell viability. Moreover, the bioactivity study revealed rapid mineralization and a higher protein adsorption rate for the monetite CP phase (M‐CP). Subsequently, the chick embryo angiogenesis assay elucidated 33% higher neovascularization for M‐CP compared with the other two CP phases. The fabricated M‐CP nanostructure constitutes a promising candidate for biomedical applications. [ABSTRACT FROM AUTHOR]

Yield=92% (232 mg); Colorless oil; HRMS (ESI-TOF) I m i / I z i : [M+H] SP + sp calcd for C SB 29 sb H SB 29 sb O SB 4 sb S SB 2 sb 505.1507, found 505.1510; SP 1 sp H NMR (400 MHz, CDCl SB 3 sb ): 7.72 (dd, I J i =0.8, 8.0 Hz, 1H), 7.67 (d, I J i =8.4 Hz, 2H), 7.30 (dt, I J i =1.2, 7.6 Hz, 1H), 7.25 (d, I J i =8.4 Hz, 4H), 7.17-7.07 (m, 7H), 7.00 (dd, I J i =1.2, 7.6 Hz, 1H), 6.44 (dd, I J i =1.2, 7.6 Hz, 1H), 5.37 (dd, I J i =5.6, 9.2 Hz, 1H), 4.44 (d, I J i =14.8 Hz, 1H), 3.76 (d, I J i =14.8 Hz, 1H), 3.59 (dd, I J i =5.6, 14.0 Hz, 1H), 3.35 (dd, I J i =9.2, 14.0 Hz, 1H), 2.41 (s, 3H), 2.36 (s, 3H); SP 13 sp C{ SP 1 sp H} NMR (100 MHz, CDCl SB 3 sb ): 144.7 (2x), 136.1, 134.7, 134.3, 132.9 (2x), 132.8, 129.7, 129.6 (2x), 129.5 (2x), 129.3 (2x), 129.2 (2x), 128.8, 128.6 (2x), 128.4, 128.1 (2x), 126.6, 66.5, 60.1, 36.4, 21.6, 21.5. The intermolecular desulfonylative cyclopropanation and intramolecular condensation processes provided a cascade pathway for the formation of two carbon-carbon single (C-C) bonds and one carbon-carbon double (C=C) bond. The proposed synthetic route forms two carbon-carbon single (C-C) bonds and one carbon-carbon double (C=C) bond. [Extracted from the article]

Single-crystal XRD studies of Bis(4-hydroxypyridinium) hexacholorostannate(IV) reveals that the crystal belongs to a triclinic system with Pī space group. The X-ray crystallography structure has [C5H6ON]+ 0.5[SnCl6]2− asymmetric unit. The band gap value for the hybrid is 3.92 eV estimated using the Kubelka-Munk function. The Bond valence sum (BVS) of tin was calculated as 3.95 based on the Sn-Cl bond distances, which is close to its formal oxidation state of +4. Exploration of the intermolecular interactions and the crystal packing using Hirshfeld surface analysis, derived from single-crystal XRD data, reveals the close contacts associated with strong interactions. [ABSTRACT FROM AUTHOR]

A new copper(II) complex [Cu(3,5,6-tcpa)(2,2′-bipy)Cl] (1) has been obtained through the one-pot hydrothermal reaction of copper chloride dihydrate with triclopyr (systematic name 2-((3,5,6-trichloropyridin-2-yl)oxy)acetic acid, abbreviation 3,5,6-Htcpa) and 2,2′-bipyridine (2,2′-bipy) coligands. 1 has crystallized in triclinic crystal system, P 1 ‾ space group. The central copper(II) ion displayed a distorted square–pyramidal geometry and was connected by one chlorido co-ligand (Clˉ), one 3,5,6-tcpa anionic chelator and one chelating 2,2'-bipy ligand to afford a mononuclear structure. 1 is further extended into a 3D network by the non-covalent interactions of H⋯Cl, H⋯O hydrogen bonds, aromatic π⋯π stacking together with Cl⋯Cl halogen bond interactions. The co-crystallization process, the crystal structure of 1 as well as the Hirshfeld surface analysis for 1 have been analyzed and described. In addition, the flexible conformation of phenoxy methylene group among 1, triclopyr acid and its previously reported co-crystallized compound also have been carefully compared and discussed. [ABSTRACT FROM AUTHOR]

Trimethyl({tris[(phenylsulfanyl)methyl]silyl}methoxy)silane (3), C26H32OS3Si, is a new ligand for transition-metal coordination chemistry derived from 3-bromo-2,2-bis(bromomethyl)propan-1-ol (1), C5H9Br3O, through silylation and following exchange of bromine groups with NaSPh. Silylated thioether ligand 3 crystallizes in the centrosymmetric space group C2/c. Bromomethylalcohol 1 crystallizes in the space group P̅1 in the triclinic crystal system with four molecules in the asymmetric unit. Analysis of the Hirshfeld surface shows structure-defining interactions for bromomethylalcohol 1, resulting in intermolecular hydrogen bonds between the hydroxyl groups along the a-axis direction. [ABSTRACT FROM AUTHOR]

The novel hydrazone-containing thieno[2,3-d]pyrimidine, namely, N′-(1,3-dioxo-1,3-dihydro-2H-inden-2-ylidene)-2-(4-oxo-5,6,7,8-tetrahydrobenzo[4,5]thieno[2,3-d]pyrimidin-3(4H)-yl)acetohydrazide 4 was synthesized in a very good yield from the reaction of the triketoester 1 or ninhydrin 2 with the exocyclic acetohydrazide 3 in methanol. Good-quality crystals of 4 were obtained by recrystallization of the compound from the DMF/MeOH solvent mixture. The target product 4 crystallized in the triclinic crystal system and P-1 space group. The topology analysis of molecular packing indicated that the H...H (30.4%), O...H (22.0%) and H...C (17.0%) contacts are the most dominant intermolecular interactions in the crystal of 4, while the O...H, N...H, H...C, N...C, O...C, C...C and O...O are the only contacts which have shorter interaction distances than the vdWs radii sum of the interacting atoms. The structure of 4 is optimized and the calculated structure showed good agreement with the experimental one. Additionally, MEP, HOMO, LUMO and the reactivity descriptors were calculated. [ABSTRACT FROM AUTHOR]

Herein, we report the in silico design and synthesis of two new nickel(II) coordination complexes, viz., [Ni(L1)][(PPh3)]DMF (1) and [Ni(L2)] (2), based on Schiff bases derived from the 2-hydroxy-1-naphthaldehyde moiety (where, L1H2 = (E)-3-(((5-chloro-2-hydroxyphenyl)imino)methyl)naphthalene-2-ol), (L2H2 = 2,2′-((1E,1′E)-(ethane-1,2-diylbis(azaneylylidene))bis(methaneylylidene))bis(naphthalen-2-ol)), PPh3 = (triphenylphosphine). The synthesized ligands L1H2 and L2H2 were coordinated to Ni(II) ions through the tridentate-ONO and tetradentate-N2O2 donor atoms, respectively. The newly synthesized complexes were fully characterized using X-ray crystallography analysis. The synthesized complexes (1) and (2) crystallized in the triclinic and monoclinic crystal system with the P1¯ and P21/c space group, respectively, and exhibited a square planar geometry around the Ni(II) ions. Computational approaches were employed to determine the structure–property relationship of the complexes. Hirshfeld surface analysis was also performed to investigate intermolecular interactions in the crystal systems. The strength of the interaction and 3D topology of crystal packing were visualized through an energy framework. To gain insights into the potential application of Ni(II) complexes as effective SARS-CoV-2 Omicron inhibitors, we performed the following docks (a) Ni(II) complexes with S protein from original SARS-CoV-2 (PDB ID: 7CWO), (b) Ni(II) complexes with selected Omicron targets (PDB ID: 7QTK and 7WK8) and (c) controls ivermectin and levosalbutamol with the original SARS-CoV-2 spike protein and the Omicron S proteins. The synthesized Ni(II) complexes (1) and (2) showed good docking results with the S protein of SARS-CoV-2, where the binding energies (ΔG) and respective Ki (inhibition constants) correlation values are −7.38 (3.87 μM) and −8.82 (341.77 nM), respectively. The molecular docking results revealed that the synthesized complexes (1) and (2) with the SARS-CoV-2 Omicron target protein (PDB ID: 7QTK) resulted the binding energy (ΔG) of −7.46 kcal mol−1 with an inhibition constant (Ki) of 3.39 μM and binding energy (ΔG) of −7.56 kcal mol−1 with an inhibition constant (Ki) of 2.89 μM, respectively. Similarly, the synthesized Ni(II) complexes (1) and (2) with the SARS-CoV-2 Omicron target protein (PDB ID: 7WK8) exhibited the binding energy (ΔG) and inhibition constant (Ki) of −7.03 kcal mol−1 and 7.08 μM and −7.89 kcal mol−1 and 1.64 μM, respectively. It was predicted that ivermectin shows a larger binding energy (ΔG) for S proteins compared to levosalbutamol after molecular docking. Further, in silico ADMET to predict the drug-likeness behaviour and pharmacokinetic response of the synthesized complexes was also explored. Overall, the present study suggests that nickel(II) complexes can be considered as potential therapeutic drugs against the Omicron target protein of SARS-CoV-2. [ABSTRACT FROM AUTHOR]

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 P-1 space group with a = 10.3368(6) Å, b = 11.9804(8) Å, c = 12.7250(5) Å, α = 100.904(4)°, β = 107.959(4)° and γ = 109.638(6)°. The different non-covalent interactions which contributed in the molecular packing of 6c were analyzed using Hirshfeld analysis. The molecular packing of the organic part of the crystal structure showed important O...H (7.1%), C...H (16.4%), C...C (1.6%), H...H (34.8%), N...H (8.0%) and C...N (4.0%) interactions while for the crystal solvent, the O...H (21.3%), H...H (61.2%) and N...H (8.1%) contacts are the most significant. The studied compound 6c is polar and has a net dipole moment of 5.6072 Debye based on DFT study. [ABSTRACT FROM AUTHOR]

A crystalline Cu(II) complex [Cu4(CHDA)2(phen)4(H2O)2(DMF)2].(NO3)22H2O was assembled by 1, 4-cyclohexanedicarboxylic acid (CHDA) and 1, 10-phenanthroline (phen) under ambient conditions. The single crystal x-ray diffraction studies evidenced the crystallization of the title complex (CCP) in triclinic crystal system with P-1 space group with V = 1996.94(14) Å3. The orientation of CHDA, packing nature, hydrogen bonding, π–π stacking stabilizing the structure of the complex are studied. FT-IR, SEM, TG-DSC, ESR and electronic absorption analysis were carried out. The gll and g⊥ values calculated from ESR curve confirm square pyramidal geometry of the Cu atom. Antimicrobial activity of the complex against Escherichia coli (Gram negative) and Staphylococcus aureus (Gram positive) was tested. The ability of complex toward free radical scavenging was estimated by DPPH assay. The cytotoxicity of the complex against cervical (HeLa) and lung adenocarcinoma (A549) cancer cells was estimated and IC50 values are reported. The CV measurements concluded the capability of the complex to act as an effective electro active material in the development of electrochemical sensors. [ABSTRACT FROM AUTHOR]

2-Amino-5-chloropyridinium 5-sulfosalicylate (2A5CP5S) material was synthesized, and a single crystal was grown by slow evaporation solution technique (SEST). The lattice parameters of the grown crystal were confirmed by the single-crystal X-ray diffraction (SXRD) analysis. It was a triclinic crystal system with a centrosymmetric P-1 space group. The various crystal planes were determined using powder X-ray diffraction (PXRD) analysis. The functional groups of the 2A5CP5S were identified by FTIR spectrum analysis. The dislocation density of the crystal was analyzed by chemical etching analysis. The thermal behavior of the 2A5CP5S crystal was determined by thermogravimetric and differential thermal analysis. The optical homogeneity of the crystal (thickness = 1 mm) was characterized by a birefringence study using a diode laser (532 nm). The photoconductivity was tested on a polished sample with an exposed area of 25 mm2. The optical transmittance of the grown crystal was found using UV–Vis NIR spectroscopy, it is 78% and the bandgap energy was found to be 3.35 eV. The z-scan technique was carried out using a He–Ne laser (632.8 nm) to analyze the nonlinear optical (NLO) properties. [ABSTRACT FROM AUTHOR]

The crystal structure and electronic properties of rhenium disulfide in the triclinic crystal system are investigated using density functional theory and pseudopotential theory. The calculated primitive cell parameters and angles within a local density approximation are shown to be in good agreement with the experimental data. It is established that the observed direct-gap character of rhenium disulfide is related to interband transitions at point X. The electron energy spectrum is characterized by many valleys. The electronic structure is mainly formed by the 3p- and 5d-states of sulfur and rhenium ions, respectively. The role of 5d-states increases while that of 3p-states decreases during the transition from the valence band to the conductance band. The observed structure is due to the low symmetry of the primitive cell and the numerous nonequivalent positions of its constituent ions. [ABSTRACT FROM AUTHOR]

In our group, the organic compounds 2,5-dibromoterephthalic acid (H2 L1) and 2,2'-bipyridine (L2) were used as biligands to react with zinc sulfate heptahydrate (ZnSO4 · 7H2O) and cobalt nitrate hexahydrate (Co(NO3)2 ·6H2O), respectively, using solvothermal method to obtain a zinc complex [Zn(L1)(L2) (H2O)]n (1) and a cobalt complex [Co(L1)(L2)(H2 O)]n (2). The structural characterization and properties measurement were performed by single crystal X-ray diffraction, elemental analysis, infrared spectroscopy, ultraviolet spectroscopy, fluorescence spectroscopy, thermogravimetric analysis and other tests. The results show that complex 1 is a monoclinic crystal system with onedimensional chain structure formed by the coordination of Zn2+ linking L12- and L2, each chain forming a three-dimensional network structure by regular stacking under intermolecular hydrogen bonding and π...π conjugation. Complex 2 is a triclinic crystal system with Co1 and Co1i ions linked by carboxylic acid oxygen atoms O4 and O4i on HbL1 to form a bidentate chelated ligand structural unit. A two-dimensional lattice structure is formed with Co2+ ligands connecting L21 and L2, and the layers are regularly stacked under O--H...O intermolecular hydrogen bonding and van der Waals forces to form a three-dimensional network structure. Both complexes 1 and 2 contain aromatic heterocycles, carboxyl heterocycles and nitrogen heterocycles, they have good fluorescence property and thermal stability, the maximum emission wavelengths of complex 1 and complex 2 are 345 nm and 333 nm, respectively. [ABSTRACT FROM AUTHOR]

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• The AHMP+.AMBA− compound was synthesized by the slow evaporation technique. • The present compound was characterized by SCXRD, FTIR and DFT analyses. • The O⋅⋅⋅H and H⋅⋅⋅H contacts are observed as significant interactions. • TG and DTA analyses show thermal stability up to 168 ºC of the present salt. • AHMP+.AMBA− is suitable for the fabrication of optoelectronic and photonic devices. The organic crystal (AHMP+.AMBA−) of the AHMP and AMBA organic compounds was successfully synthesized and grown by the slow evaporation solution process. The present work focuses on the crystal structure, Hirshfeld surface, spectroscopic and DFT analyses of the title salt. The crystal geometry of AHMP+.AMBA− monohydrated salt was characterized by the single-crystal XRD technique. The synthesized salt crystallizes in the triclinic crystal system and P-1 space group. The identification of the functional groups of the compound has been done by FTIR spectroscopy and DFT/B3LYP-D3/6–311++ G (d,p) level of theory. Further, Hirshfeld surface mapping and its associated two-dimensional fingerprint plots predict that the O⋅⋅⋅H and H⋅⋅⋅H interactions are dominant for stabilizing the crystal structure. TG-DTA reveals the crystal is thermally stable up to 168 ºC. The optical studies have been performed by the time-dependent DFT (TD-DFT) and UV–Vis spectroscopic methods. Moreover, the Z-scan experiment has been done to obtain third-order NLO properties. Additionally, the HOMO-LUMO energy gap, MEP maps and theoretical NLO parameters have also been calculated. [Display omitted] [ABSTRACT FROM AUTHOR]

4-(2-amino-2-oxoethyl) phenyl 4-methylbenzenesulfonate (APMBS), a novel compound, has been synthesized and characterized by spectro-analytical techniques. X-ray diffraction data reveals it crystallizes in the triclinic crystal system with space group P1¯\documentclass[12pt]{minimal}\usepackage{amsmath}\usepackage{wasysym}\usepackage{amsfonts}\usepackage{amssymb}\usepackage{amsbsy}\usepackage{mathrsfs}\usepackage{upgreek}\setlength{\oddsidemargin}{-69pt}\begin{document}$$P\overline{1}$$\end{document}. The structure is stabilized through strong N–H⋯O, weak C–H⋯O and C–H⋯π hydrogen bond interactions yielding a supramolecular structure. The N1A–H1AA⋯O4A, C4–H4⋯O3, and C14–H14⋯Cg1 (Ring: C8–C13) interactions link the molecules into dimers, while the interaction C9-H9–O2 results in the formation of a molecular chain along the a-axis. The optimized structural geometry, by and large, as calculated using DFT and HF techniques is in conformity with the corresponding X-ray data. The DFT computation further aid in the follow up investigations including frontier molecular orbitals (FMOs), density of states (DOS), atomic charges, and molecular electrostatic potential surface (MEP). For a comprehensive description of various molecular intersections, Hirsheld surface and fingerprint plots analysis has been reported, besides the combined atoms-in-molecules (QTAIM) and reduced density gradient (RDG) analysis. Docking studies have been performed against the target protein Tubulin-Colchicine: Stathmin-Like Domain Complex.Graphical Abstract: 4-(2-amino-2-oxoethyl) phenyl 4-methylbenzenesulfonate (APMBS), a novel compound, has been synthesized and characterized by spectro-analytical techniques. X-ray diffraction data reveals it crystallizes in the triclinic crystal system with space group P1¯\documentclass[12pt]{minimal}\usepackage{amsmath}\usepackage{wasysym}\usepackage{amsfonts}\usepackage{amssymb}\usepackage{amsbsy}\usepackage{mathrsfs}\usepackage{upgreek}\setlength{\oddsidemargin}{-69pt}\begin{document}$$P\overline{1}$$\end{document}. The structure is stabilized through strong N–H⋯O, weak C–H⋯O and C–H⋯π hydrogen bond interactions yielding a supramolecular structure. The N1A–H1AA⋯O4A, C4–H4⋯O3, and C14–H14⋯Cg1 (Ring: C8–C13) interactions link the molecules into dimers, while the interaction C9-H9–O2 results in the formation of a molecular chain along the a-axis. The optimized structural geometry, by and large, as calculated using DFT and HF techniques is in conformity with the corresponding X-ray data. The DFT computation further aid in the follow up investigations including frontier molecular orbitals (FMOs), density of states (DOS), atomic charges, and molecular electrostatic potential surface (MEP). For a comprehensive description of various molecular intersections, Hirsheld surface and fingerprint plots analysis has been reported, besides the combined atoms-in-molecules (QTAIM) and reduced density gradient (RDG) analysis. Docking studies have been performed against the target protein Tubulin-Colchicine: Stathmin-Like Domain Complex. [ABSTRACT FROM AUTHOR]

Alkaline earth saccharinates Mg - Ba were synthesized by the known solution-based methods and also by mechanochemical synthesis. The compounds were characterized by TG/DSC, X-ray powder diffraction, and Mg, Ca and Ba saccharinates by single-crystal X-ray analysis. The structure of Mg(sac)2 ·7H2O (sac = saccharinate), is known but the diffraction data were collected at 170 K in this study for comparison with other structures. Crystals of hydrates of Ca - Ba saccharinates are very thin needle-like. A 4 µm crystal of Ca(sac)2 ·7H2O gave a low intensity diffraction pattern of sufficient quality to locate non-hydrogen atoms (triclinic crystal system, space group P-1, Z = 4). Crystals of strontium saccharinate were too thin for data collection, however the formula Sr(sac)2 ·4H2O, proposed in a previous publication was confirmed by thermogravimetric analysis. Diffraction from a 12 µm thick crystal of Ba(sac)2 ·4.5H2O resulted in a complete data set (monoclinic crystal system, space group P2/c, Z = 8). In the corresponding structures, the Mg ion is six-coordinated forming an octahedron, both Ca ions are irregularly eight-coordinated with the polyhedra bridged by saccharinate ions into chains, whereas both Ba ions are irregularly nine-coordinated with the polyhedra sharing edges and corners through bridging water molecules and bridging saccharinate ions into double chains. All water molecules are included into hydrogen bonding into layers with only van der Waals and weak C-H···O bonds between the chains. [ABSTRACT FROM AUTHOR]

Coordination-driven self-assembly of nickel (II) ions with equimolar amounts of 1, 10 phenanthroline, and benzoic acid was used to create homonuclear nickel (II) MOF-type supramolecule. Single crystal X-ray diffraction, scanning electron microscopy, differential scanning calorimetry, photoluminescence measurement, FT-IR, UV-visible spectroscopy, and nitrogen physisorption measurement were used to characterize the compound. The single crystal X-ray diffraction study reveals that the synthesized compound is twodimensional with pores in the structure. The homonuclear nickel (II) MOF-type supramolecule crystallized in a triclinic crystal system, with space group P-1 (No.2) and unit cell parameters a = 9.2053(4) Ǻ, b = 13.2964(5) Ǻ, c = 15.8998(6) Ǻ, α = 66.296(2) °, β = 89.400(2) °, γ = 89.441(2) °. The crystal structure result shows π- π and intermolecular interactions between adjacent 1, 10-phenanthroline molecules. DSC result showed a gradual decomposition confirming thermal stability of the compound. The emission (468 nm) spectrum result shows energy peaks of a typical multiphonon phase, indicating luminescence process. The surface topology and single absorption maximum at 308 nm reveal formation of a distorted octahedral structure. Brunauer–Emmett–Teller and Langmuir surface area results 383.741 and 975.830 m² g–1, respectively, indicate high adsorption capacity. Langmuir isotherm model result of the compound shows an efficient adsorption property for storing energy. The excellent nickel (II) MOF-type supramolecule adsorption capacity and emission property opened the door to its use in energy storage applications especially in photovoltaic cells. [ABSTRACT FROM AUTHOR]

Self‐assembly of (((1‐(pyridin‐2‐yl)ethylidene)hydrazono)methyl)phenol ligand (L1) and MnCl2 proceeded with the hydrolysis of the ligand affording the new [Mn(L2)Cl2]n 1D coordination polymer where L2 is 2‐(1‐hydrazonoethyl)pyridine. The structure of [Mn(L2)Cl2]n was confirmed using FTIR, CHN, and X‐ray diffraction of single crystal. It crystallized in the triclinic P‐1 crystal system with a = 7.0697(9) Å, b = 8.878(1) Å, c = 9.402(2) Å, α = 113.99(2)°, β = 95.48(1)°, γ = 111.77(1)°, and V = 479.13(15) Å3. The Mn(II) is octahedrally coordinated with two nitrogen atoms from L2 and four chloride ions. The chloride anions act as bridging ligand that connect the Mn(II) centers leading to the formation of the 1D polymer. Based on continuous shape (CShM) measure tool, the coordination configuration is closer to the octahedron rather than a trigonal prism. Using Hirshfeld analysis, the Cl ... H (29.2%), H ... C (13.6%), and C ... C (3.7%) contacts are the most important in the molecular packing of [Mn(L2)Cl2]n complex. The ligand L2 has better antibacterial, antifungal, and antioxidant activities than the Mn(II) complex. The [Mn(L2)Cl2]n complex has higher cytotoxic effect than L2 against both lung carcinoma A‐549 and lung fibroblast MRC‐5 cell lines. The IC50 and CC50 values of the Mn(II) complex are 26.09 ± 1.76 and 60.40 ± 3.74 μg ml−1, respectively, while 121.23 ± 5.91 and 241.13 ± 13.29 μg ml−1, respectively, for L2. [ABSTRACT FROM AUTHOR]