A terbium 2,6-naphthalenedisulfonic acid compound, [Tb(H2O)9]Cl(C10H6O4S4)2 (C10H6O4S42− = 2,6-naphthalenedisulfonate), is prepared and characterized by single-crystal X-ray diffraction. This compound is characterized by an isolated structure with the terbium ion possessing a mono-capped square antiprism coordination geometry. The [Tb(H2O)9]3+ cations and (2,6-naphthalenedisulfonic acid)2− anions are linked by hydrogen-bonding interactions to yield a three-dimensional supramolecular network. The solid state luminescence spectrum reveals that this compound shows the strongest emission band in the red region. The luminescence emission peaks can be ascribed to the characteristic emissions of the 4f electron intrashell transitions 5D4 → 7F5, 5D4 → 7F4 and 5D4 → 7F2 of the Tb3+ ion. The CIE (Commission Internationale de L’Eclairage) chromaticity coordinates are (0.5647, 0.4338). Solid-state UV/Vis diffuse reflectance spectra reveal that compound 1 shows a wide optical band gap of 4.92 eV.
A novel terbium 2,6-naphthalenedisulfonic acid compound is prepared and characterized
Three new cyanide-bridged heterobimetallic complexes {[Cu(L)]2[Cr(CN)5(NO)]}ClO4·2H2O (1), {{[Cu(cyclam)][Fe(CN)5(NO)]}·H2O}n (2), {{[Cu(cyclam)]3[Cr(CN)5(NO)]2}·CH3OH·4H2O}n (3) (L=2,12-dimethyl-3,7,11,17-tetraazabicyclo [11.3.1] heptadeca-1 (17), 13, 15-triene, cyclam=1,4,8,11-tetraazacyclodecane) have been successfully assembled from the pentacyanometalates and two copper(II) compounds and characterized by elemental analysis, IR spectroscopy and X-ray structure determination. X-ray structural analysis revealed that the Complex 1 is a cationic trinuclear CrCu2 entity with the positive charge balanced by ClO4− ion, while complexes 2 and 3 were structurally characterized showing a 1D chain. The magnetic properties of the reported cyanide-bridged complexes have been experimentally studied and theoretically simulated, disclosing the ferromagnetic interaction between the Cr(I) ion and the Cu(II) ion through the cyanide bridge.
The crystal structure of the thiosemicarbazide derivative 4-cyclohexyl-1-(thiophene-2-carbonyl)thiosemicarbazide (ChtcTSC), C12H17N3OS2, is reported here. The title compound ChtcTSC has been characterized by various physicochemical techniques viz UV–Vis., Infrared, and NMR. It crystallizes in the monoclinic system having space group P21/c. The dihedral angle between the thiophene and cyclohexyl rings is 60.7(4)°. The crystal packing is established by intermolecular N–H⋯O packing interactions involving a three-center donor hydrogen bond between the keto oxygen atom of the thiophene group and H atoms belonging to the hydrazine group which links the molecules into chains along the (011) plane of the unit cell. Hydrogen bonds between the hydrazine hydrogen atom and one of the thiophene groups and C–H⋯Cg π -ring interactions provide added stability to the crystal packing. The fingerprint plots associated with Hirshfeld surface analysis indicate that there are different types of weak interactions viz. O⋯H–C, O⋯H–N, and S⋯H–C. The geometry optimization has been performed using the DFT method, and geometrical parameters thus obtained for ChtcTSC correlate with the single-crystal X-ray data. The TD-DFT study showed a small HOMO and LUMO energy gap of 2.869 eV. The electronic transition from the ground state to the excited state due to a transfer of electrons from HOMO to LUMO levels is mainly associated with the n → π* transition.
The crystal structure of 4-cyclohexyl-1-(thiophene-2-carbonyl)thiosemicarbazide (ChtcTSC) is reported here where the title compound ChtcTSC has been characterized by various physiochemical techniques including UV–Vis., Infrared, NMR, DFT and Hirshfeld surface analysis.
Two new hybrid solids viz. {Hpz}2[H7CrMo6O24]·6H2O (1) and [Co(2-Hampz)2Cl4] (2) have been crystallized via solvent evaporation technique using pyrazole (pz) and 2-aminopyrazine (2-ampz) respectively. The solids were characterized using single crystal X-ray diffraction, fourier transform infrared spectroscopy, elemental analysis, scanning electron microscopy and thermal analysis. The solid 1 crystallized in orthorhombic system with space group Pbca, a = 23.1796(8), b = 11.1281(4), c = 25.1499(9) Å, Z = 8. The solid 2 crystallized in triclinic system with space group P-1, a = 7.1986(5), b = 7.3917(5), c = 7.8896(6) Å, α = 115.758(3), β = 110.450(3), γ = 96.904(3)°, Z = 1. While, solid 1 is a new Anderson–Evans cluster based solid, 2 is a new pseudopolymorph of cobalt complex [Co(2-ampz)4Cl2]. Crystal structure analysis suggested that supramolecular interactions facilitate the crystal packing in solids 1 and 2. In addition, the role of synthetic parameters in dictating the nature of self-assembly of solids 1 and 2 in aqueous medium has also been analyzed.
An Anderson–Evans cluster based solid, {Hpz}2[H7CrMo6O24]·6H2O (1) and a new pseudopolymorph of cobalt complex [Co(2-ampz)4Cl2] viz. [Co(2-Hampz)2Cl4] (2) have been synthesized using pyrazole (pz) and 2-aminopyrazine (2-ampz) respectively.
The crystal structure of NH4[Zn(cma)(H2O)2]·H2O (cma3– = N-carboxymethylaspartate(3–)) is determined by single crystal X-ray structure analysis. The orthorombic crystals (P212121, a = 7.7901(4) Å, b = 11.2368(4) Å, c = 13.2048(5) Å, α = β = γ = 90°, Z = 4) were obtained from the reaction mixture in the form of racemic conglomerate. The single crystal X-ray structure analysis revealed the maximum deviation of bond angles around the Zn atom from an ideal octahedral geometry 14.09° with ∑ = 67.23° and Θ = 236.69°. Intermolecular interactions are based mainly on a moderate N–H⋯O and O–H⋯O hydrogen bonds. The structure shares similar structural features with other structures containing aspartates and their derivatives as a ligands. The results of using different HAR methods based on semi-empirical (B3LYP) and non-empirical (PBE0) global hybrid GGA DFT functionals were compared.
The crystal structure of NH4[Zn(cma)(H2O)2]·H2O (cma3– = N-carboxymethylaspartate(3–)) is determined by single crystal X-ray structure analysis. The orthorombic crystals (P212121, a = 7.7901(4) Å, b = 11.2368(4) Å, c = 13.2048(5) Å, α = β = γ = 90°, Z = 4) were obtained from the reaction mixture in the form of racemic conglomerate.
Abnormal carbene complex of Pd(L1)2, where L1 = 1,3-Bis(2,6-diisopropylphenyl)-2,4-diphenylimidazole and normal carbene complex of Pd(L2)2, where L2 = 1,3-dimesityl-4,9-dioxonaphtho-2,3-diimidazole were prepared from a Pd(0) precursor Pd(COD)(CH2TMS)2. Both the complexes crystalize in the triclinic space group P-1 and cell parameters of Pd(L1)2 and Pd(L2)2 are a = 12.0477 Å, b = 17.5269 Å, c = 18.9786 Å, α = 114.4855°, β = 92.5295°, γ = 107.9472° and a = 11.5007 Å, b = 15.2316 Å, c = 17.9007 Å, α = 67.061°, β = 72.143°, γ = 72.183° respectively. In both case N-heterocyclic ligands are distorted towards palladium direction. Further, crystal structures reveal that the palladium atom is covalently bonded to the two aNHC and nNHC ligands respectively. The electrochemical properties of these complexes were determined by cyclic voltammetry analysis in THF solution under argon atmosphere. The enunciated reversibility of the complexes can be explained by sequential one electron oxidations of the palladium centre from Pd(0) to Pd(I) and then Pd(II).
Abnormal carbene complex of Pd(L1)2, where L1 = 1,3-Bis(2,6-diisopropylphenyl)-2,4-diphenylimidazole and normal carbene complex of Pd(L2)2, where L2 = 1,3-dimesityl-4,9-dioxonaphtho-2,3-diimidazole were prepared from a Pd(0) precursor of Pd(COD)(CH2TMS)2. The crystal structures were determined by single crystal X-ray diffraction data and electrochemical properties were also determined by cyclic voltammetric analysis.
A new coordination polymer of coper (II), [tetra-azido)tris(2-pyridyl)amine)dicopper(II)] (1) has been synthesized by the reaction between copper(II) nitrate hexahydrate, sodium azide and tris(2-pyridyl)amine under solvothermal conditions in aqueous methanol. The structure has been characterized by single-crystal X-ray diffraction. An analysis of Hirschfeld surfaces was examined. Single-crystal results reveals that the structure contains two independent copper(II) centers, both having approximately square pyramidal coordination: in one, two of the basal sites are occupied by bidentate tris-(2-pyridyl)amine and two azido ligands, with a third azido ligand at the apical site, while the other center is coordinated only by azido ligands. All azido ligands bind two copper centers, forming a coordination polymer chain with two types of Cu2N2 rings and one type of Cu4N4 ring, and in which all azido ligands form a bridge between two metal centers in mode µ-1,1. The Hirshfeld analysis revealed an azido··· (pyridyl) interaction in the coordination polymer chain, as well as weak C-H···N interactions, one of which links the chains into sheets.
A new dinuclear copper (II) polymer [tetra-azido(tris(2-pyridyl)amine)dicopper(II)] (1) has been synthesized under solvothermal conditions and been characterized by single-crystal X-ray diffraction and Hirshfeld surface analysis.
The molecular structure of (1)
Reactions of two dialkyl-substituted pyrazine ligands with a triosmium cluster are described. Both 2-ethyl-3-methylpyrazine (C4H2N2MeEt) and 2,5-dimethylpyrazine (C4H2N2Me2) react with the labile triosmium cluster [Os3(CO)10(NCMe)2] at 80 °C to afford [HOs3(CO)10(µ-C4HN2MeEt)] (1) and [HOs3(CO)10(µ-C4HN2Me2)] (2), respectively. Clusters 1 and 2 are formed via C–H bond activation at the α-carbon of the corresponding pyrazine ligand. Cluster 2 reacts with PPh3 at room temperature in the presence of Me3NO‧2H2O to yield the mono- and diphosphine-substituted clusters [HOs3(CO)9(PPh3)(µ-C4HN2Me2)] (3) and [HOs3(CO)8(PPh3)2(µ-C4HN2Me2)] (4), respectively, both of which exist in more than one isomeric form in solution. All new clusters have been characterized using spectroscopic methods together with single-crystal X-ray diffraction studies for 1, 2, and 4. The bonding in these clusters have been investigated by electronic structure calculations.
Two new triosmium clusters bearing a metalated pyrazineligand have been synthesized and structurally characterized.The reactivity of one of these newly synthesized clusters towards PPh3 has also been investigated.
The title compound is synthesized, and characterized by spectroscopic and XRD methods. The compound crystallizes in the orthorhombic crystal system with the space group P212121. The structure exhibits C–H⋯N intermolecular interaction and π⋯π interactions. Hirshfeld surface analysis was performed to determine the individual contributions of intermolecular contacts to the crystal packing. The structural and electronic properties of the molecule were investigated by density functional theory method with B3LYP hybrid functional. Intramolecular interactions involved in the crystal structure was analyzed through topological atom-in-molecules analysis and noncovalent interactions method. Molecular electrostatic potential surface shows the chemical reactive regions around the nitrogen and hydrogen atoms.
The article presents the characterization of synthesized compound by single crystal X-ray diffractionmethod. Atom-in-molecules analysis and noncovalent interactions Intramolecularinteractions involved in the crystal structure were analyzed by DFT method.
京公网安备 11010802042870号
京ICP备2023020795号-1
扫码关注我们
求助内容：
应助结果提醒方式：