Synthesis and crystal structure of a new cesium barium borate,CsBaB3O6

A new ternary borate oxide, cesium barium borate, CsBaB₃O₆, has been synthesized by solid-state reaction at 700 °C, and the single crystals were grown using CsF as a flux. The crystal structure has been determined by X-ray diffraction. It crystallizes in the trigonal space group P321 with a cell of dimensions a=12.469(3)Å, c=7.444(3)Å, α=90.00°, γ=120.00°, V=1002.3(5)ų, Z=6. The fundamental building units of CsBaB₃O₆ are the B₃O₆ plane hexagonal rings, which are parallel to each other and stack along the c-axis, and the Cs and Ba atoms alternately occupy sites between the B₃O₆ sheets. A comparison of the structures of CsBaB₃O₆, β-BaB₂O₄ and CsBO₂ is presented.     

Synthesis,crystal structure and properties of a new congruently melting compound,K3ZnB5O10

A new compound, K₃ZnB₅O₁₀, has been synthesized by solid-state reaction. It crystallizes in the monoclinic system, space group P2₁/n with unit–cell parameters a = 7.6391(5) Å, b = 19.2304(13) Å, c = 7.6905(5) Å, β = 116.698(4)° and Z = 4. The structure of the compound is solved by the direct methods and refined to R1 = 0.0286 and wR2 = 0.0600. K₃ZnB₅O₁₀ contains a two-dimensional ZnB₅O₁₀ layer, which forms by connecting isolated double ring [B₅O₁₀] groups and ZnO₄ tetrahedra. The K atoms filling in the interlayer and intralayer link the layers together. Functional groups presented in the sample were identified by FTIR spectrum. UV–vis–NIR diffuse reflectance spectrum exhibits ultraviolet cutoff edge is about 190 nm. The DSC analysis proves that K₃ZnB₅O₁₀ is a congruently melting compound.     

Synthesis, growth, structure and characterization of a new semiorganic crystal

A new semiorganic single crystal, tris(allylthiourea)silver(I) nitrate was grown from an aqueous solution containing silver(I) nitrate and allylthiourea by slow evaporation solution growth technique at room temperature. The crystal belongs to trigonal system with centrosymmetric space group R3 and the cell parameters are, a = 12.5090(4) Å, b = 12.5090(4) Å, c = 21.7130(8) Å, V = 3348.89 Å³, and Z = 6. The various functional groups present in the molecule are confirmed by Fourier transformed infrared spectroscopy. High transmittance is observed in the visible region and band-gap energy is calculated by Kubelka–Munk algorithm. The structure and the crystallinity of the materials were further confirmed using powder X-ray diffraction analysis. Microhardness studies were also carried out to elucidate the mechanical behavior. Thermogravimetric and differential thermal analysis reveal the purity of the sample and no decomposition is observed up to the melting point.     

Synthesis,crystal structure and non-linear optical properties of a new cyanide-containing compound

Reaction of K₃[Fe(CN)₆], NiCl₂ and diethylenetriamine (dien) resulted in the formation of a cyanide-containing heterometallic compound [Ni(dien)₂]₂[Fe(CN)₆]·4H₂O 1. The structure consists of two octahedral [Ni(dien)₂]²⁺ cations, one octahedral [Fe(CN)₆]^4? anion and four crystallization water molecules, which are held together by hydrogen-bonding interactions. Its TG curve exhibits two stages of mass loss. Compound 1 in DMF solutions has a very strong third-order non-linear optical (NLO) behavior with an absorption coefficient and refractive index α₂?=?1.10?×?10^?11?m?w^?1, n ₂?=??3.05?×?10^?19?m²?w^?1, respectively, and third-order NLO susceptibility χ⁽³⁾ 4.34?×?10^?13?esu.     

Synthesis, crystal structure, and nonlinear optical properties of Li6CuB4O10: a congruently melting compound with isolated [CuB4O10]6- units

Single crystals of Li(6)CuB(4)O(10) have been synthesized, and its crystal structure has been determined. Li(6)CuB(4)O(10) crystallizes in the non-centrosymmetric triclinic space group P1 (No. 1). The structure consists of isolated [CuB(4)O(10)](6)(-) polyanions that are bridged by six LiO(4) tetrahedra. Li(6)CuB(4)O(10) is a congruently melting compound. It produces SHG intensity similar to that produced by KH(2)PO(4) and is phase-matchable.     

Preparation and crystal structure of Li6Zr2O7 and Li6Hf2O7

Li₆Zr₂O₇ was obtained by annealing an intimate mixture of LiOH · H₂O and freshly prepared ZrO₂ in a stream of argon. It is monoclinic: C2/c, a = 1 044.5(1), b = 598.9(1), c = 1 020.0(1) pm, β = 100.26(1)°, Z = 4, R = 0.016 for 1 218 F values and 55 variables. The structure is closely related to that of NaCl with an ordered distribution of the metal atoms on the sodium sites while the oxygen atoms occupy seven eighths of the chlorine positions. Li has square pyramidal, Zr octahedral oxygen coordination. The corresponding Hf compound is isotypic: a = 1 040.2(1), b = 596,2(1), c = 1 015.0(1) pm, β = 100.36(1)°. ⁷Li nuclear magnetic resonance spectra of this compound give no indication for a high mobility of the Li⁺ ions.     

Synthesis, crystal structure and properties of a charge-transfer compound [(CH3)3CNH3]3[PMo12O40] · 2H2O

A charge-transfer compound [(CH₃)₃CNH₃]₃[PMo₁₂O₄₀] · 2H₂O was synthesized and characterized by IR, UV, ESR, diffusion reflectance electronic spectrum, cyclic voltammogram and X-ray crystallography. Oxygen atoms of the polyoxometalate anion, N atoms of organic substrates (CH₃)₃CNH₂ and O atoms of water molecules are involved in hydrogen bonding. The solid reflectance electronic spectra and IR data indicate the presence of interaction between the [PMo₁₂O₄₀]³⁻ and the organic substrates in the solid state. Photosensitivity to ultraviolet light was assessed for the compound, showing that charge-transfer resulted from oxidation of the organic substrates and the reduction of the heteropolyanion.     

3,4-二羟基苯甲酸镉配合物的合成,结构表征及荧光性质

采用碳酸镉和3,4-二羟基苯甲酸、2,2’-联吡啶合反应得到了配位聚合物[Cd(C7H5O4)2·(H2O)3·2H2O(1).采用元素分析、红外光谱、荧光光谱对配合物进行了表征.用X射线单晶衍射仪测定了配合物的晶体结构.配合物为单斜晶系,P2(1)/c空间群,昌胞参数Z=4,a=0.78338(8)nm,b=1.98...     

Monoclinic honeycomb-layered compound Li3Ni2SbO6: preparation, crystal structure and magnetic properties

Two synthetic routes-ion-exchange preparation from layered Na(3)Ni(2)SbO(6) at 300 °C and direct solid-state synthesis at 1150 °C resulted in layered Li(3)Ni(2)SbO(6), a cation-ordered derivative from the rocksalt type. The Fddd form reported earlier could not be reproduced. According to the XRD Rietveld analysis, Li(3)Ni(2)SbO(6) is a pseudohexagonal monoclinic structure, C2/m, with a = 5.1828(2) ?, b = 8.9677(3) ?, c = 5.1577(2) ?, β = 109.696(2)°. No Li/Ni mixed occupancy was detected. At high temperatures, the magnetic susceptibility follows the Curie-Weiss law with a positive value of Weiss temperature, ～8 K, indicating a predominance of ferromagnetic interactions. However, Li(3)Ni(2)SbO(6) orders antiferromagnetically at T(N)～ 15 K. The effective magnetic moment is 4.3 μ(B)/f.u. which satisfactorily agrees with theoretical estimations assuming high-spin configuration of Ni(2+) (S = 1). Electron spin resonance (ESR) spectra show single Lorentzian shape line attributed to Ni(2+) ion in octahedral coordination. The absorption is characterized by isotropic temperature independent effective g-factor g = 2.150 ± 0.005. In accordance with the layered honeycomb crystal structure determined for Li(3)Ni(2)SbO(6), the superexchange interaction between Ni(2+) ions through Ni-O-Ni pathways within Ni(2)SbO(6) layers are assumed to be ferromagnetic, while the dominant interaction between layers is antiferromagnetic.     

Crystal structure of a new lithium indium borate Li3InB2O6

Single crystals of synthetic Li₃InB₂O₆ were obtained by heating a mixture of Li₂CO₃, In₂O₃ and B₂O₃; its formula was determined by the resolution of the structure from X-ray diffraction data. The compound is monoclinic, space group P2₁/n; the unit cell parameters are a=5.168(5) Å, b=8.899(9) Å, c=10.099(10) Å, β=91.112(17)°; Z=4. The crystal structure was solved from 669 reflections until R=0.0249; it exhibits a three-dimensional framework of vertex-sharing InO₅ trigonal bipyramids and BO₃ triangles, which isolates Li ions in channels. This structure is characterized by unusual oxygenated environments of In cations and of one of the three Li cations, which are forming more or less regular trigonal bipyramids. This compound melts incongruently at 827 °C; the powder may be obtained by annealing at 750 °C a mixture of Li₂CO₃, In₂O₃ and B₂O₃.     

Synthesis,characterization, crystal structure,and antibacterial evaluation of Ni (II) complex with new dithiophosphorus compound

The reaction of 2,4-bis (4-methoxyphenyl)-1,3,2,4-dithiadiphosphetane-2,4-disulfide (Lawesson^’s reagent) with phenylethylamine produced [H₃NCH₂CH₂C₆H₅]⁺ [(C₆H₅CH₂CH₂NH)(p C₆H₄OMe)PS₂]^? (1). Furthermore, reaction of 1 with NiCl₂ in dry methanol led to the novel complex 2. The compounds were characterized by ¹H and ³¹P NMR, IR spectroscopy, and elemental analysis. A single crystal X-ray structure of complex 2 showed that the nickel complex is square planar. The complex formed a supramolecular structure via intermolecular S1…H7B and O1…H2N2 hydrogen bonds. The X-ray crystallography of complex showed [R²₂](18) and R⁴₄(18) motifs in the monomers were connected to each other via S1…H7B, O1…H2N2 hydrogen bonds with donor–acceptor distance of 2.89 and 2.51 Å, respectively. The new compounds were additionally tested in view of their antibacterial properties.     

A new noncentrosymmetric vanadoborate: synthesis, crystal structure and characterization of K2SrVB5O12

A new noncentrosymmetric vanadoborate compound, K(2)SrVB(5)O(12), is synthesized by the high temperature solution method. It crystallizes in the monoclinic space group P2(1) (no. 4) with lattice constants a = 6.618(3) ?, b = 8.378(4) ?, c = 9.974(5) ?, β = 99.789(6)°, Z = 2. The structure consists of vanadoborate anionic layers with K(+) and Sr(2+) cations filling the void spaces via electrostatic interactions to form the three-dimensional network. The TG-DSC curves and the UV-Vis-NIR diffuse reflectance spectrum were measured. Band structures and density of states were calculated. The powder second harmonic generation (SHG) effect of K(2)SrVB(5)O(12) is similar to that of KH(2)PO(4) (KDP).     

Synthesis,characterization, and crystal structure of a new truly one-dimensional compound: PV2S10

PV₂S₁₀ was obtained by heating the elements in stoichiometric proportions at 490°C in evacuated Pyrex tubes. The crystal symmetry is monoclinic, space group $\text{P2}{}_1\text{c}$, with the unit cell parameters a = 12.734(8)Å, b = 7.349(7)Å, c = 23.662(4)Å, β = 95°22(1), V = 2205(4)ų, and Z = 8. The structure was solved from 2269 independant reflexions, and anisotropic least squares refinement gave R = 0.036 with 236 variables. The structure can be described as made of [V₂S₁₂] units forming endless chains themselves linked, two by two, by [PS₄] tetrahedra. In these units each vanadium is surrounded by eight sulfur atoms (mean d_VS = 2.459Å) arranged in a distorted bicapped triangular prism. Two of these prisms shared a rectangular face to form [V₂S₁₂] groups, in which intercationic distances implied vanadium-vanadium bonds (mean d_VV = 2.852(2)Å). Between the infinite double chains, only SS weak van der Waals' bonds exist. More than two thirds of the sulfur atoms are present as [SS]^?II pairs, (mean d_SS = 2.015Å); the rest are S^?II anions.     

Synthesis,properties and crystal structure of a heteropoly compound containing titanium

K4H2CoW12O40·2TiO2·9H2O crystallizes from an aqueous solution of Na2WO4, Co(OAc)2 and Ti(SO4)2. The compound has very similar i.r. and u.v. spectra to those of [CoW12O40]6– and [CoW11TiO40]8– but its polarographic behaviour is different from that of [CoW11TiO40]8– and exhibits only reduction of tungsten(VI). A single crystal structural analysis indicates that this compound consists of the heteropolyanion [CoW12O40]6–, titanium–oxygen chain, potassium ions and water molecules.     

Synthesis,crystal structure and properties of a quaternary oxide with a new structure type,BiGaTi4O11

A new quaternary oxide, BiGaTi₄O₁₁ (bismuth gallium tetratitanium undecaoxide), was prepared by heating a mixture of the binary oxides at 1373 K in air. BiGaTi₄O₁₁ melts at 1487 K and prismatic single crystals were obtained from a sample melted at 1523 K and solidified by furnace cooling. The structure of BiGaTi₄O₁₁ was analyzed using single‐crystal X‐ray diffraction to be of a new type that crystallized in the space group Cmcm. A Bi³⁺ site is coordinated by nine O^2? anions, and three oxygen‐coordinated octahedral sites are statistically occupied by Ga³⁺ and Ti⁴⁺ cations. A relative dielectric constant of 46 with a temperature coefficient of 57 ppm K^?1 in the temperature range 297–448 K was measured for a polycrystalline ceramic sample at 150 Hz–1 MHz with a dielectric loss tan δ of less than 0.01. Electrical resistivities measured at 1073 K by alternating‐current impedance spectroscopic and direct‐current methods were 1.16 × 10^?4 and 1.14 × 10^?4 S cm^?1, respectively, which indicates that electrons and/or holes were conduction carriers at high temperature. The optical band gap estimated by the results of diffuse reflectance analysis was 2.9–3.0 eV, while the band gap obtained from the activation energy for electrical conduction was 3.5 eV.     

Synthesis,spectroscopic, thermal,crystal structure properties,and characterization of new Hofmann-Td-type complexes with 3-aminopyridine

In this study, synthesis of two new tetracyanocadmate(II) and tetracyanozincate(II) complexes based on 3-aminopyridine (3AP) and investigation of their structural properties were reported. These complexes were characterized by using vibration spectroscopy, elemental, thermal analysis and single crystal X-ray diffraction (SC-XRD) techniques. Investigation of the elemental, spectral and single crystal data of these complexes showed that the formulas [Cd(3AP)₂Zn(μ₄-CN)₄]_n (1) and [Cd(3AP)₂Cd(μ₄-CN)₄]_n (2) fully explained their crystal structure. General information about the structural and chemical properties of these complexes obtained in single crystal form was obtained by observing the changes in the characteristic peaks of the 3AP with the [Zn(μ₄-CN)₄]^2- and [Cd(μ₄-CN)₄]^2- structures that make up these complexes. The behaviors of these complexes against changes in temperature were obtained by examining the temperature-dependent changes of their mass. The asymmetric unit of the heterometallic complexes 1 and 2 consist of half Cd(II) ion, half M ion [M = Zn1 in 1 and Cd2 in 2], two cyanide ligands and one 3AP.     

Synthesis, growth, crystal structure and characterization of a new organic material: glycine glutaric acid

Glycine glutaric acid, a new organic compound has been synthesized and good quality single crystals were grown by slow evaporation technique. The structure of the grown crystal was elucidated by using single crystal XRD. The presence of the functional groups was confirmed by using FT-IR spectroscopy. The optical transparency was studied by using UV-vis spectrophotometer and it was found that the crystal is having high optical transparency. The thermal stability of the crystal was studied by using thermo-gravimetric and differential thermal analyses and found that it is stable up to 150°C. The room temperature dielectric studies were also carried out over the wide frequency range: 10 mHz to 10 MHz.