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In the current research work, we investigated the growth of the new potassium arsenate tellurate material formulated as K2(HAsO4).Te(OH)6 (KAsTe) through the use of the slow preparation method. The (KAsTe) compound crystallized in the monoclinic system with centrosymmetric space group P21/c. Within this structure, two types of polyhedra (Te-O6 and HAsO4) were observed in the presence of K+ cations. The stability and the cohesion of the crystal structure were ensured by the linkage of different polyhedra via O‒H...O hydrogen bonds. To locate the closest contacts within this crystal structure, Hirshfeld surface analysis was performed. In fact, according to the fingerprint plots, we inferred that the hydrogen bonds constitute the dominant interactions present within this structure. The vibrational spectroscopy study at room temperature unveiled the occurrence and the independence of the ionic groups and provided detailed data on hydrogen bonds present in the crystal lattice. Thermal analyses (DSC, DTA, TG and MS) proved the presence of three phase transitions at 445, 514 and 555 K and indicated that no mass loss was recorded before 460 K. Furthermore, the σdc variation performed on (KAsTe) material suggested an important level of conductivity at high temperature, associated with the motion of H+ proton. This behavior goes in good agreement with the presence of the super‒ionic protonic phase transition at 445 K. [ABSTRACT FROM AUTHOR]

The synthesis of 1-(4(tert-butyl)-4-methoxy-[1,1-biphenyl]-4-yl) ethenone (4TBMBE) has been realized in excellent yield by using 4-tert-butyl phenylboronic acid and 1-bromonitrobenzene as the reactants. The single crystals were obtained by solvent-loss technique and its characterization was carried out using the spectral and X-ray diffraction methods. The molecule crystallizes in the monoclinic crystal system with space group (P21/c). There exists one C–H...O intramolecular and an intermolecular C–H···π interaction, besides one π···π (Cg···Cg) interaction responsible for stabilizing the unit cell molecular packing. The density functional theory has been employed to optimize the structure and to carry out the HOMO/LUMO analysis, computation of reactivity parameters, molecular electrostatic potential map and Mulliken population analysis. The Hirshfeld surface analysis probes the existence of various interactions in the crystal structure. Crystal voids analysis confirmed the absence of any significant cavity within the crystal packing. The relative contribution for each contact has been analyzed using the 2D fingerprint plots and their favourability has been validated by the enrichment ratio. The 3D topology of molecular packing has been visualized using energy framework analysis and the nature of molecular interactions existing within the structure has been ascertained using NCI-RDG analysis. The molecular docking investigations have been performed to study the anti-inflammatory action of 4TBMBE against the p38 MAP kinase inhibitor. [ABSTRACT FROM AUTHOR]

A new hybrid compound, (C5H14N2)[MnCl3(H2O)3]Cl, 1, was grown by slow evaporation from an aqueous solution at room temperature. The X-ray diffraction analysis revealed that the compound crystallizes in the monoclinic space group P21/n. The crystal structure of the Mn(II) complex is characterized as an alternation of 0-Dimensional organic chains and inorganic layers linked together by N/O–H···Cl hydrogen bonds which lead to three-dimensional supramolecular architecture. The thermal decomposition was studied by TGA techniques and Electronic properties such as HOMO and LUMO energies were calculated. The gap energy value can classify this compound among the semiconductors. Magnetic measurements indicate that the compound exhibits extremely weak antiferromagnetic interactions. In the crystal, the molecules are connected by Mn–OH2···Cl and Mn–OH2···Cl–Mn, N–H···Cl–Mn and N–H···H2O–Mn hydrogen bonds into a three-dimensional supramolecular entity. The Hirshfeld surface analysis revealed that the dominant interactions are: Cl···H/H···Cl (54.0%), H···H (41.5%), and O···H/H···O (4.5%). [ABSTRACT FROM AUTHOR]

A novel compound (1E,1′E)-N,N′-(ethane-1,2-diyl)bis(1-(5-nitrothiophen-2-yl)methanimine) [EDNM] was synthesized from thiophene derivative in view to get multidentate ligand with potential biological activity. EDNM is characterized by FT-IR, 1H and 13C NMR and UV–Vis spectroscopic techniques and confirmed by SCXRD. EDNM crystallizes in the monoclinic system with P21/c space group with Z value 4 and unit cell parameters a = 5.6540(3) Å, b = 17.9249(8) Å and c = 7.5077(5) Å. DFT was employed for theoretical evaluations using B3LYP with the basis set 6–311 + + G (d,p). Geometry optimization, vibrational analysis, NMR, electronic absorption, MEP, FMO, Mulliken charges and NBO analysis were performed, thereby establishing the nature of reactive sites, band energy gap and atomic charges of EDNM. Theoretical values matched well with the experimental findings. NBO analysis revealed the donor acceptor interactions in molecule. Analysis of global reactivity descriptors along with Fukui indices outlines the elaborate scheme of reactive sites of the molecule, and Hirshfeld surface investigation revealed the intermolecular interactions in crystal packing. [ABSTRACT FROM AUTHOR]

Thiosemicarbazides are sulfur-based nitrogen-rich donor ligands, characterized by π-delocalized electronic charge and flexible molecular chain. The flexible molecular chain and polydentate nature is responsible for their wide biological and synthetic profile to synthesize several classes of heterocycles. In this context, the molecular and crystal structures coupled with Hirshfeld surface (HS) analysis of benzylidene thiosemicarbazides: (E)-2-(4-hydroxybenzylidene) hydrazine-1-carbothioamide, (3a) and (E)-2-(3-nitrobenzylidene) hydrazine-1-carbothioamide, (3b) are reported. Consequently, single crystal x-ray revealed interesting results, and the analyzed compounds were found to be polymorphs of the previously reported structures each having widely different unit cell. Briefly, compound (3a) crystallized with a single molecule in the asymmetric unit whereas its polymorph has six. In contrast, compound (3b) crystallized with Z = 2 having single molecule in asymmetric unit of the polymorph. Subsequently, HS analysis successfully visualized, explored, and quantified weak interactions present in the crystal lattices of the polymorphs. HS analysis revealed oxygen atoms of the nitro group significantly influence HS of molecule (3b). [ABSTRACT FROM AUTHOR]

The molecular structure of Schiff base ZIm was investigated using spectroscopic (NMR, UV–vis) techniques. Theoretical calculations of the mentioned compound have been carried out using density functional theory at the B3LYP/6-31G(d) level of theory. Geometrical parameters such as bond lengths (Å) and angles (°) obtained by DFT calculations show excellent agreement with X-ray analysis result. The Hirshfeld surface (HS) analysis shows the different percentage interactions: H/H (49.8%), H/C (28.7%), N/H (15.2%) and O/H (5.7%) interactions. The 1H and 13C NMR chemical shifts with respect to TMS were calculated using the gauge-independent atomic orbital (GIAO) method in CDCl3 and compared with the experimental data. The UV–Vis spectrum of ZIm was computed with the B3LYP and CAMB3LYP functionals and the 6-31G(d) basis set in different solvents such as CHCl3, CH3CN, MeOH and DMSO. The frontier molecular orbital's (FMO's) analysis and molecular electrostatic potential surface (MEP) were investigated using theoretical calculations. The theoretical results show good agreement with the experimental results. [ABSTRACT FROM AUTHOR]

From an aqueous solution of (MoVI–MnIV–CH3COOH), an orange crystal was isolated, which consists of Waugh-type polyoxometalate K3(NH4)3[MnMo9O32]·9H2O (I). Its structure is established by single-crystal X-ray diffraction, IR spectroscopy and UV–Vis absorption. Thermogravimetric analysis and cyclic voltammetry measurement were also reported. Compound (I) crystallizes in the Trigonal system, R32 space group with a = 15.747 (8) Å, b = 15.747 (6) Å, c = 12.377 (6) Å, γ = 120° (8), V = 2657.9 (3) Å3, and Z = 3. We can see in (I), a pair of enantiomers, originated from the homochiral Waugh-type polyoxometalate building units, which are further interact with the potassium ions forming two kinds of alternately arranged 2D polymeric sheets. The whole is linked by hydrogen bonding interactions through ammonium ions and water molecules to form a three-dimensional supramolecular structure. The prevalence of these interactions is illustrated by Hirshfeld surface analyses. Results of cations sensing of Cu2+, Ni2+, Cd2+, Fe2+, Mg2+ and Pb2+ by K3(NH4)3[MnMo9O32]·9H2O are also investigated in this work. [ABSTRACT FROM AUTHOR]

The tetrapropylammonium tetrabromidoantimonate (III) [(C3H7)4N][SbBr4] is a new member of the organic–inorganic hybrid family like perovskite system. This compound crystallizes in the orthorhombic centrosymmetric Pbca space group at room temperature. Its structure can be described by an alternation of organic and inorganic layers parallel to the (001) plan, made up of [(C3H7)4N]+ cations and [SbBr4]− anions. An extensive network of hydrogen bonds ensures the interconnection of the different entities. Greater knowledge on these interactions has been provided based on the Hirshfeld surface analysis and 2D fingerprint plots. The differential scanning calorimetry studies disclose a presence of two phase transitions located at T1 = 343 K and T2 = 363 K. The temperature dependence of the Raman spectra of [(C3H7)4N][SbBr4] single crystals was studied in the wavenumber range from 10 to 3500 cm−1 for temperatures between 303 and 380 K. The strong evolutions of the Raman shift, half-widths and intensity of many lines associated with the organic cation [(C3H7)4N]+ were observed with discontinuities in the vicinity of the two phase transitions, especially for the lines 1024 cm−1and 1053 cm−1, respectively. The Nyquist plot (− Z" vs. Z') from the complex impedance spectrum showed only one semicircular arc, representing the grain effect in the electrical conduction. The thermal evolution of the conductivity of the grains also presents an Arrhenius-type behavior, revealing that charge carriers have to overcome different energy barriers while conducting and relaxing. [ABSTRACT FROM AUTHOR]

This paper deals with the crystal structure of two new non-centrosymmetric hybrid compounds obtained from an aqueous solution by slow evaporation method and characterized by various techniques mainly single-crystal X-ray diffraction. In the atomic arrangement of 2-methylbenzylammonium chloride (1), the organic cations and the chloride anions are linked to each other via N–H...Cl hydrogen bonds; organic cations in zigzag distribution along b-axis in z = 0 and z = ½ are also close enough to enable a C–H...π interaction to occur. In 3-methylbenzylammonium chloride (2), the organic cations are linked together by C–H...π interactions and through N–H...Cl and C–H...Cl hydrogen bonds to form a two-dimensional network. To support experimental results, DFT calculations have been accomplished via the B3LYP method and 6-311++G(d,p) basis set on molecular geometry, vibrational, and electronic properties. The non-covalent interactions were studied quantitatively using the Hirshfeld surfaces (HS) associated with 2D fingerprint plots. The NLO properties have been also investigated by DFT and compared to the urea reference. [ABSTRACT FROM AUTHOR]

A new salt Bis(o-xylylenediammonium) tetrachloride monohydrate, denoted by OXDACl, produces a novel organic–inorganic compound with centrosymmetric property, prepared by slow evaporation technique in an aqueous solution. This one has been assumed a pattern in the orthorhombic Pnma space group, and the following crystallographic parameters obtained are a = 9.0677(9) Å, b = 24.282 (2) Å, c = 9.4726 (8) Å, V = 2085.7 (3)Å3 and Z = 4, at 150 K. It is investigated by X-ray diffraction, fluorescence, infrared, and UV–visible spectroscopy. The crystal wrap is endorsed by the O–H···Cl, N–H···Cl hydrogen bond interactions among the organic network and the inorganic one, which stabilize the crystal packing. Besides to get a perception into the attitude of these interconnections, Hirshfeld surfaces analysis have been scrutinized. Computational calculations were performed, employing density functional theory (DFT), and were made by comparison with the experimentally determined structure to examine the molecular structure with geometrical optimization, vibrational, and topological parameters of OXDACl by B3LYP/6–311 + + G(d,p) basis. [ABSTRACT FROM AUTHOR]

Synthesis, crystal structure and spectroscopic characterization of the new Cd(II) complex with the bidentate ligand 4,4'-dimethyl-2,2'-dipyridine (DMDPy), [CdI2(DMDPy)2], is reported. The cadmium cation is hexa-coordinated in a distorted octahedral configuration by four nitrogen atoms of two DMDPy ligands and two iodide anions. In the structural arrangement of the title compound, the different chemical entities are arranged in planes around z = n ± ¼. Intermolecular interactions were investigated by Hirshfeld surface and contact enrichment tools. Mulliken charge distribution, molecular electrostatic potential maps and HOMO/LUMO energy gaps were computed. Infrared spectroscopy was used to verify the functional groups present in the compound and to study their vibrational behavior in the crystalline state. [ABSTRACT FROM AUTHOR]

In this work, we are interested to study the Hirshfeld surface analysis and fingerprint plots to identify the significant intermolecular interactions in the lattice. The NMR spectroscopy of 13C and 31P is in agreement with the X-ray structure. The UV–visible spectrum exhibits a strong absorption with the band gap energy (Eg) values are equal to 2.28 eV and 2.67 eV for indirect and direct method, respectively. A dielectric measurement of this material has been realized in the frequency range (200 Hz–5 MHz). The order–disorder phase transition mechanism, observed at 338 K, is probably due to the dynamics of [(C4H9)4P]+ cations. The activation energies values obtained from the conductivity are: Ea1 = 0.79 eV (T < 338 K), and Ea2 = 1.27 eV (T > 338 K). [ABSTRACT FROM AUTHOR]

The new organic cyclohexaphosphate (C6H7ClFN)4 (Li)2(P6O18)(H2O)4, has been synthesized at room temperature by an acid/base reaction between H6P6O18 and 3-chloro-4-fluoroaniline as an organic template. The crystal structure of (C6H7ClFN)4 (Li)2(P6O18)(H2O)4 was solved by single crystal X-ray diffraction analysis. A double head-to-head layer of cations is formed by hydrophobic interactions. Hirshfeld surface analysis reveals the nature of intermolecular contacts of the title compound. The contacts enrichment ratio shows that both strong electrostatic interactions and hydrophobic contacts are overrepresented. This hybrid material was then characterized by 1H, 13C, 31P, 15N and 19F solid-state NMR and IR spectroscopies. Electrical conductivity was also studied using impedance spectroscopy and results showed that the conductivity at 105 °C was equal to 96.5 × 10−4 S.cm−1. Antioxidant properties of this compound were studied, in vitro, at various concentrations with different tests; 1,1-diphenyl-2-picrylhydrazyl (DPPH), ferric reducing power (FRAP), Trolox equivalent antioxidant capacity (TEAC) or ABTS+, using 6-hydroxy-2,5,7,8-tetramethylchroman-2-carboxylic acid (Trolox) as control. [ABSTRACT FROM AUTHOR]

The chemical preparation, characterization by single-crystal X-ray diffraction, elemental analysis and IR spectroscopy of the new Fe(III) complex (C5H7.50N3O)2[FeCl4] are reported. The Fe(III) cation is four-coordinated, in tetrahedral fashion, by four chlorine atoms. The [FeCl4]− tetrahedra are located parallel to the (a, b) plane at z = ¼ (2n + 1) between layers of organic cations (C5H7.50N3O)2+. The FeCl4 moieties are inserted between these planes by establishing N–H...Cl and C–H...Cl hydrogen bonds generated by amino and methyl groups as donors and Cl− anions as acceptors to form a three-dimensional network. The organic groups are linked together by N–H...N hydrogen bonds to form chains extending along the [110] direction. These chains are arranged in planes parallel to (a, b) at z = ½n. Intermolecular contacts on the Hirshfeld surface were investigated statistically. The most favored and stabilizing contacts are the strong (N–H...Cl−, N–H...N) hydrogen bonds as well as the weaker ones C–H...Cl−. The vibrational absorption bands were identified by infrared spectroscopy. Electronic properties such as HOMO and LUMO energies were also derived. [ABSTRACT FROM AUTHOR]

New derivatives of phosphoramido acid with the formula(C6H11NCH3)(NHCOCF3)P(O)(O−)(CH3–+NH2–C6H11)(1) (amidophosphoricacid), (C6H5)2P(O)(O−)(+NH3–C6H4–NH2)(2) (phosphonicacid), (C6H5O)2P(O)(O−)(+NH3–C6H4–NH2) (3) (phosphoricacidester) were synthesized and characterized by X-ray crystallography. The asymmetric unit of compounds 1–3 consists of one molecule with the P atom in a tetrahedral environment. The X-ray structural analysis showed that the H-bond patterns depend on the kind of atoms linked to the P atom. In the crystal packing of compound 1, P(O)···H–N and C(O)···H–N hydrogen bonds in 3 and P(O)···H–N distances in compounds 2 and 3 led to a one-dimensional arrangement. The energy of P–O···H–N hydrogen bond (EHB) model and stabilizing energies (E2) were calculated. Hirshfeld surface analysis demonstrated that the C···H contact is attributed to CH···π contact in the 2 and 3 compounds and the F···H contact is referred to hydrogen bond in one O···H counterion interaction. Quantitative structure–activity relationship (QSAR) was used to comprehend the relationship between molecular structural features and the inhibitory of investigated compounds. The use of density functional theory along with the QSAR model for enzymes revealed the importance of QH parameter in describing the anti-AChE and anti-urease activities of monophosphoramidates including P(O)–NH2 moiety. [ABSTRACT FROM AUTHOR]

New hybrid arsenotungstates based on Dawson polyanions [C4H7N2]6[As2W18O62]·4H2O (1) have been isolated by conventional solution method and characterized by single-crystal X-ray diffraction, infrared spectrum and UV-visible spectroscopies and thermogravimetric analysis. Hirshfeld surface analysis was performed to study the intermolecular interactions. Compound 1 crystallizes in hexagonal system, in a P-3 space group, with cell parameters a = 20.2904(2) Å, b = 20.2904(2) Å, c = 16.8246(2) Å, and a V = 5998.38(11) Å3. Compound 1 exhibits a three-dimensional chain constructed from Well-Dawson anions linked together with (C4H7N2)+ cations and water molecules. [ABSTRACT FROM AUTHOR]

The 3-amino-1,2,4-triazole (atz)-based manganese complex was prepared and characterized through single-crystal X-ray diffraction, IR, EPR, and UV-visible spectroscopy. In the crystal structure, individual complex are interconnected through N(O)-H…Cl hydrogen bonds into 1D undulating chains running parallel to the [110] direction of the unit cell. Chains further grow into 2D supramolecular layers by way of the lattice water molecules of coordination and the chloride anions (O-H…Cl). Layers pack along the b-axis of the unit cell mediated by O-H…Cl(N) and N-H…O(Cl) hydrogen bonds forming a 3D supramolecular architecture. The theoretical calculations were also performed to optimize the structure of the complexes in the gas phase to confirm the structures proposed by X-ray crystallography. In addition, IR and UV-visible spectra of complex were calculated and compared with the corresponding experimental spectra to complete the experimental structural identification. The three-dimensional Hirshfeld surface (3D-HS) and their relative two-dimensional fingerprint plots (2D-FP) reveal that the structure is dominated by H…Cl/Cl…H (50.5%), H…O/O…H (11.3%) and N…O/O…N (10.2%) contacts. [ABSTRACT FROM AUTHOR]

Hirshfeld surfaces and two-dimensional fingerprint plots are used to visualize and analyse intermolecular interactions in two new organotin(IV)-phosphoryl complexes: [Sn(CH)[OP(O)(OCH)]] (I) and {[(4-CH)CHNH][CH(4-CH)N]P(O)}Sn(CH)Cl (II). In (I), the asymmetric unit is composed of the Sn(CH)[OP(O)(OCH)] segment bonded to the neighbouring segment through Sn-O bonds thus constructing a coordination polymer. The tin centre has an Sn[C][O] environment with the axial positions occupied by methyl groups and with the oxygen atoms of Sn-O bonds located at the equatorial plane, while the oxygen atoms of OCH groups do not take part in the coordination interaction. In (II), the asymmetric unit contains one complete molecule and the tin centre has an Sn[C][Cl]O trigonal bipyramid coordination environment, where the phosphoric triamide ligand and one of the chlorine atoms are placed in axial positions. Hirshfeld surface analysis on the asymmetric unit of (I) shows a contribution of 5.9 % of total interactions in crystal for Sn...O contacts related to involving of four-coordinated Sn site of asymmetric unit with two oxygen atoms of two neighbouring phosphates in the coordination polymer. The Sn centre in the asymmetric unit of (II) receives a second interaction from chlorine atom that, however, has negligible contribution portion in the total interactions (evaluated by fingerprint plot) in the crystal. On the other hand, this chlorine affects the geometry at the Sn atom and causes the open C-Sn-C bond angle (of 140.18(24)°). For both structures, the contribution of H...H contacts to the total interaction is decisive, being 59.1 % for (I) and 73.9 % for (II); so that the one distinct spike observed in each of the fingerprint plots is related to H...H contacts. The O...H (34.1 %) in (I) and the H...Cl (20.2 %) in (II) are the characteristic intermolecular contacts in the corresponding structures, monitoring as two pairs of H-bond spikes for O...H and two sharp spikes for H...Cl. Furthermore, the structure (I) does not show the C...H interaction, whereas (II) including unsaturated carbon atoms manifests such interaction (5.7 %) as two very short spikes. [ABSTRACT FROM AUTHOR]