Growth and characterization of semiorganic NLO crystal of l-glutamic acid hydrochlorobromide (LGHCB)

Single crystals of nonlinear optical material l-glutamic acid hydrochlorobromide (LGHCB) were grown by slow evaporation technique from its aqueous solution. Optically good quality crystals of dimension 20 × 10 × 2 mm³ were obtained. The lattice parameters for the grown crystals were determined using single crystal X-ray diffraction study. The LGHCB crystal belongs to non-centrosymmetric P2₁2₁2₁ space group. The crystal structure was resolved by direct method and refined by full matrix least-square method using SHELXL-97. Using the powder X-ray diffraction study, the crystallinity of the grown crystal was confirmed and the diffraction peaks are indexed. From Fourier transform infrared spectroscopy study, the various functional groups present in LGHCB crystal were elucidated. The UV–Vis-NIR absorption spectrum was recorded in the range of 200–2,000 nm, and the lower cut off wavelength is ~235 nm. Optical band gap of the grown crystal was found to be 5.22 eV. Thermal properties of LGHCB crystal were studied by thermogravimetric analysis and derivative thermogravimetric analysis. The second harmonic generation efficiency of LGHCB crystal was confirmed by Kurtz’s powder technique.     

Crystal growth, structural, thermal, and dielectric characterization of Tutton salt (NH4)2Fe(SO4)2·6H2O crystals

A good quality single crystal of Tutton salt, (NH₄)₂Fe(SO₄)₂·6H₂O, with dimensions 6 × 7 × 3 mm³ was successfully grown by the slow evaporation growth technique at ambient temperature. The grown crystal was subjected to single crystal X-ray diffraction study which confirms that the grown crystal is monoclinic in nature with the space group P2₁/c. Optical absorption spectrum reveals that the grown crystal has good optical transparency in the entire visible region and its energy band gap was determined. The thermal behavior of the grown crystal was investigated by thermogravimetric and differential thermal analysis. The dielectric measurements were carried out to determine the dielectric behavior of the crystal.     

Synthesis,growth, structure and characterization of nickel(II)-doped hexaaquacobalt(II) dipotassium tetrahydrogen tetra-o-phthalate tetrahydrate crystals

Single crystals of K₂[Co_(1−x)Ni_x(H₂O)₆] (C₈H₅O₄)₄·4H₂O (x = 0.25) (PCNHP), a semiorganic black colored transparent crystal of size ∼20 × 13 × 4 mm³, are grown from an aqueous solution of potassium hydrogen phthalate enriched with cobalt chloride and nickel chloride by slow evaporation solution growth technique at room temperature. Structural analysis by single crystal X-ray diffraction reveals that the crystal belongs to monoclinic system with space group P2₁/c and the cell parameters are a = 10.41(3) Å, b = 6.84(2) Å, c = 29.46(9) Å, Z = 4. Incorporation of both Co(II) and Ni(II) into the potassium hydrogen phthalate (KHP) crystal lattice is well confirmed by EDS and chemical tests. Powder XRD profiles indicate the crystallinity and FT-IR studies reveal the vibrational patterns. The UV–vis optical absorption spectrum of PCNHP shows the lower optical cut-off at ∼300 nm and the crystal was transparent in the entire visible region. The crystalline perfection of the grown crystal analysed by high-resolution X-ray diffraction (HRXRD) analysis reveals that the diffraction curve (DC) contains multi-peaks with low angular spread indicating the possibility of low angle structural grain boundaries. Scanning electron microscope (SEM) studies indicate the structure defect centers. The dielectric, thermal and mechanical behaviors of the specimen were also investigated.     

Synthesis of polycrystalline materials of SrWO4 and growth of its single crystal

The polycrystalline materials of SrWO₄ were synthesized by means of a solid phase reaction with analytical purity SrCO₃ and WO₃ at high temperature. The transparent SrWO₄ single crystal with dimension of ϕ 22 mm×40 mm has been successfully grown along a-axis by Czochralski method. X-ray powder diffraction results show that the as-grown SrWO₄ single crystal belongs to tetragonal system and I4₁/a space group. The measured density of SrWO₄ is 6.439 g·cm⁻³ by buoyancy method. The effective segregation coefficients of W and Sr elements in SrWO₄ single crystal are close to 1 by the X-ray fluorescence method. __________ Translated from Journal of Shandong University (Natural Science), 2005, 40(4) (in Chinese)     

Synthesis and characterization of a novel η 2-iminoacyl monocyclopentadienyl titanium(IV) complex

An unusual complex, [CpTi(η²-(C,N)-2-ArNH–C₆H₄C=NAr)Cl₂] (Ar?=?2,6- ⁱ Pr₂C₆H₃) (1) has been synthesized and characterized by elemental analysis, NMR spectra, and single crystal X-ray diffraction. The ¹³C NMR resonance of the imine carbon atom of 1 at δ?221?ppm is consistent with the η²-(C,N) binding. This was confirmed by single crystal X-ray diffraction study of 1. In the complex, Ti atom is five-coordinate with a η²-bound iminoacyl ligand and one Cp ligand occupying the axial position in a distorted square pyramid.     

CsPdCl3 – eine Verbindung mit [Pd2Cl6]-Baugruppen und anorganischem Kation

CsPdCl₃ – A Compound with Isolated [Pd₂Cl₆] Groups and an Inorganic Cation The crystal structure of CsPdCl₃ has been characterized by X-ray powder diffraction methods. Meanwhile it was possible to isolate single crystals and to confirm the structure by single crystal X-ray investigations. CsPdCl₃ crystallizes orthorhombic in space group Ibam (No. 72) with a = 13.724(1), b = 10.579(1), c = 8.499(1) Å, and Z = 8. CsPdCl₃ is a compound with a dinuclear [Pd₂Cl₆]^2– group and a cesium cation. Formerly such groups are only found in combination with large “organic” cations so far.     

First examples of η1-ligated halogenophosphaalkenes. Crystal structures of trans-[RhCl(PPh3)2{η1-PXC(SiMe3)2}] (X = F or Cl)

Syntheses and single crystal X-ray diffraction studies of the η¹-halogenophosphaalkene complexes trans-[RhCl(PPh₃)₂{η¹-PXC(SiMe₃)₂}] (X = F, Cl) are reported.     

Crystal growth,spectral characterization and structural studies of a luminescent coordination polymer of calcium(II) complex of benzilic acid

Single crystals of a new calcium(II) complex of benzilic acid, [Ca(C₁₄H₁₁O₃)₂(C₁₄H₁₂O₃)₂] have been successfully grown by gel diffusion technique at room temperature. Single crystal X-ray diffraction study reveals that the compound belongs to orthorhombic system with space group Fddd. The adjacent CaO₈ units are linked via O–H–O interaction to form one dimensional polymeric chains. The extensive hydrogen bonding interactions lead to a supramolecular structure. The grown crystals were further characterized by elemental analysis, FT-IR, UV–Visible, thermogravimetric, powder X-ray diffraction and solid state photoluminescence studies.     

Growth and characterization of 2-amino-4-picolinium toluene sulfonate single crystal

2-Amino-4-picolinium toluene sulfonate (2A4PTS), a new organic material, was synthesized and grown as single crystals in room temperature by slow evaporation solution growth technique using water as solvent. The crystal structure of 2A4PTS has been determined using single crystal X-ray diffraction studies. 2A4PTS belongs to monoclinic crystal system. The molecular arrangements in the crystal were studied. The structural perfection of the grown crystals has been analysed by high-resolution X-ray diffraction (HRXRD) rocking curve measurements. Fourier transform infrared (FTIR) spectral studies have been performed to identify the functional groups. The optical transmittance window and the lower cutoff wavelength of the 2A4PTS have been identified by UV–Vis–NIR studies. The nonlinear optical properties have been investigated by Z-scan method. The nonlinear refractive index and linear absorption coefficient of the 2A4PTS are found to be in the order of 10⁻⁸ cm²/W and 10⁻⁴ cm/W, respectively. The laser induced surface damage threshold for the grown crystal was measured using Nd:YAG laser. Thermal analysis carried out on the compound reveals that 2A4PTS is stable up to 133 °C. The microhardness test was carried out and the load dependent hardness was measured.     

Synthesis and characterization of a new organic nonlinear optical crystal: l-Phenylalaninium maleate

l-Phenylalaninium maleate (abbreviated as LPM) chemical formula C₉H₁₂NO₂⁺·C₄H₃O₄⁻, a new organic nonlinear optical crystal was grown by slow evaporation technique. Transparent needle shaped crystal of dimensions 7 mm × 1 mm × 0.5 mm was obtained. Single crystals of LPM have been subjected to X-ray diffraction analysis to estimate the lattice parameters and the space group. The powder X-ray diffractogram of the crystal has been recorded and the reflections from various planes are identified. The XRD studies confirm the crystalline nature. The qualitative analysis on the crystal has been carried out using Fourier transform infrared (FTIR) and Fourier transform Raman (FTRaman) spectral measurements. The presence of hydrogen and carbon in the grown crystal was confirmed by using proton and carbon nuclear magnetic resonance (NMR) spectral analyses. Optical behaviour of the crystal was investigated using UV–vis spectroscopy. The thermal stability of the crystal was analysed with the aid of thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The nonlinear optical (NLO) property of the crystal was tested by Nd:YAG laser source.     

Crystal growth, spectral, optical, and thermal characterization of glycyl-l-alanine hydrochloride (GLAH) single crystal

A new semi-organic nonlinear optical material glycyl-l-alanine hydrochloride (GLAH) was grown successfully by slow evaporation solution growth method. The solubility of GLAH was estimated for a wide range of temperatures. Large size single crystal of size 15?×?9?×?6?mm³ was grown at room temperature. The grown crystal was subjected to single crystal X-ray diffraction study which confirms that the grown crystal is monoclinic in nature with the space group P2₁. The molecular weight of the title compound was estimated by mass spectrometry. Functional groups and the modes of vibrations were identified by FT-IR spectral analysis. The UV?Cvisible spectral study reveals that the percentage of optical transmission of the sample is very high in the entire visible and UV regions. The second harmonic generation of the crystal was confirmed by the Kurtz and Perry technique. The hardness of the sample was tested by microhardness test which shows that the grown crystal belongs to the soft category of materials. The thermal stability of the compound was studied by TG?CDTA analyses which indicate that the crystal is thermally stable up to 248.6?°C.     

Growth and Thermal,Electrical, Structural Characterization of Mixed Hydrated Single Crystal

Mixed single crystal was made by mixing saturated aqueous solutions of NiSO₄ · 6H₂O and CuSO₄ · 5H₂O by volume (80:20) and the mixture was kept to form the crystals at room temperature by slow evaporation process. After some days, big pieces of greenish blue, dark colored crystals were grown. To determine the weight of NiSO₄ · 6H₂O and CuSO₄ · 5H₂O in the crystal, Ni-DMG complexiometrical and EDTA gravimetrical analysis was done respectively. From this analysis it was concluded that 5.8 molecules of water of crystallization is present in the mixed single crystal. The crystals were characterized by UV-Visible, FTIR and single crystal X-ray diffraction studies. From single crystal XRD lattice parameters have been calculated. All these structural analysis confirms formation of new single crystal. Further, DTA-TGA, dc electrical conductivity and dielectric constant studies were done from the room temperature to 400 °C.From DTA studies it was observed that 5.8 molecules of water of crystallization get dehydrated in four major steps at temperature 115 °C, 150 °C, 240 °C and 325 °C respectively corresponding to the detachment of 1 mole, 3 moles, 1 mole and 0.8 mole of water of crystallization. DC electrical conductivity and dielectric constant studies also show close agreement to the dehydration steps. The observed peaks in the conductivity verses temperature graph have been explained on the basis of release of water molecules and subsequent dissociation of these released water molecules into H⁺ and OH⁻ ions.     

Synthesis,structures and Hirshfeld surface analysis of Ni(II) and Co(III) complexes with N2O donor Schiff base ligand

Two octahedral complexes [NiL(HL)]ClO₄.0.5CH₃OH and [CoL₂]ClO₄ have been synthesized with N₂O donor Schiff base ligand {((2-(phenylamino)ethyl)imino)methyl}phenol (HL) and characterized by spectroscopic techniques and single crystal X-ray diffraction studies. The molar conductivities data of the two complexes show that the complexes are 1:1 electrolyte. Single crystal X-ray diffraction data shows both Ni(II) and Co(III) complexes have distorted octahedral geometry and two ligands are coordinated to the metal centers and one ClO₄⁻ ion outside the coordination sphere. The intermolecular interactions in the complexes are evaluated by Hirshfeld surface analysis and revealed a significant contribution of non- or weakly polar interactions to the packing forces for both molecules, with crystal structure of Co(III) complex featuring short H/H contacts.     

Synthesis and X-ray structure of 1,1-dimethylhydrazinium azide

1,1-Dimethylhydrazinium azide, [ (CH₃)₂NH–NH₂] [N₃], was prepared in high yield from 1,1-dimethylhydrazine and HN₃ in CH₂Cl₂ solution at −20°C. The new compound has been fully characterized by elemental analysis, multinuclear NMR (¹H, ¹³C, ¹⁴ N, ¹⁵ N) and vibrational spectroscopy (IR, Raman). The structure in the solid state was determined by a low temperature (173 K) single crystal X-ray diffraction analysis.     

Growth and characterization of thiosemicarbazide hydrochloride: a semiorganic NLO material

Thiosemicarbazide hydrochloride (TSCHCL) was synthesized by mixing thiosemicarbazide and hydrochloride in 1:1 molar ratio in double distilled water. Single crystals of TSCHCL were grown by slow evaporation at room temperature and were characterized by single crystal X-ray diffraction study to determine the molecular structure and by FT-IR, ¹H and ¹³C NMR spectral analyses to confirm the synthesized compound. Thermogravimetric and differential thermal analyses reveal the thermal stability of the crystal. The transmission spectrum of TSCHCL showed that the crystal is transparent in the wavelength range 380–1100 nm. High resolution X-ray diffractometry (HRXRD) was employed to evaluate the perfection of the grown crystal. Mechanical properties of the grown crystal were studied using Vickers microhardness test. Second harmonic generation efficiency of the powdered TSCHCL was tested using Nd:YAG laser and is ∼1.5 times that of potassium dihydrogen orthophosphate.     

Synthesis and Crystal Structure of a New Alkali Metal Tantalum Sulfide: Na3TaS4

Needle-shaped, moisture sensitive, yellow crystals of Na₃TaS₄ were obtained by the reaction of Na₂S₃, Ta, and S at 450 °C. The structure was determined by single crystal X-ray diffraction and refined to R1 and wR2 values of 0.0172 and 0.0381, respectively. Na₃TaS₄ crystallizes with 32 formula units in the orthorhombic space group Fdd2 (No.: 43) with a = 27.113(4), b = 28.326(6) and c = 7.918(1) Å. The structure consists of discrete tetrahedral TaS₄^3– ions and Na⁺ ions.     

A Series of Polyoxometalate-Viologen Photochromic Materials for UV Probing,Amine Detecting and Inkless and Erasable Printing

In this work, by using two kinds of viologen ligands three POM-based Compounds were obtained under hydrothermal conditions, namely [Ag^I(bmypd)_0.5(β-Mo₈O₂₆)_0.5] (1) (bmypd ⋅ 2Cl=1,1′-[Biphenyl-4,4′-bis(methylene)]bis(4,4′-bipyridyinium)dichloride), [Ag^I₂(bypy)₄(HSiW₁₂O₄₀)₂] ⋅ 14H₂O (2) and [Ag^I(bypy)(γ-Mo₈O₂₆)_0.5] (3) (bypy⋅Cl=1-Benzyl-4,4′-bipyridyinium chloride). The structures were characterized by Fourier transform infrared spectroscopy (FT–IR), Powder X-ray diffraction (PXRD), X-ray photoelectron spectroscopy (XPS) and single crystal X-ray diffraction. Compounds 1–3 show excellent photochromic ability with fast photoresponse under the irradiation of ultraviolet light with different degrees of color changes. So compounds 1–3 can be used as visible ultraviolet detectors. Compounds 1–3 also possess photoluminescence properties with fast and excellent fluorescence quenching effect. Compounds 1–3 also can be used as inkless and erasable printing materials with suspensions of 1–3 applied to filter paper. Compounds 1–3 can also produce color changes in amine vapor environment, especially in an NH₃ atmosphere. Compounds 1–3 can be used as organic amine detectors.     

Growth, spectral, and thermal characterization of semicarbazone of p-hydroxy acetophenone (SPHA)

A new organic nonlinear optical material semicarbazone of p-hydroxy acetophenone (SPHA) was synthesized. Good quality single crystal of SPHA was successfully grown by slow evaporation method at room temperature. The crystal system was identified and lattice dimensions were measured from the single crystal X-ray diffraction (XRD) analysis. The various planes of reflection were identified from the powder XRD pattern. The presence of functional groups was qualitatively found by Fourier transform infrared (FTIR) spectral analysis. The proton and carbon nuclear magnetic resonance (¹HNMR and ¹³CNMR) spectral studies confirmed the presence of hydrogen and carbon bonded network in the grown crystal. The UV?CVisible absorption spectrum was recorded to study the optical transmittance in the range from 200 to 800?nm. The thermal stability of compound was determined by thermogravimetric and differential thermal analysis (TG-DTA) traces. The existence of second harmonic generation (SHG) signal was observed using Nd:YAG laser with fundamental wavelength of 1064?nm.     

Spin crossover in iron(II) complexes with tris(pyrazol-1-yl)methane

Mononuclear iron(II) coordination compounds with tris(pyrazol-1-yl)methane (HC(Pz)₃) described as [Fe{HC(Pz)₃}₂]A₂ × nH₂O, where A = Cl⁻, Br⁻, I⁻, 1/2 SO₄²⁻, n = 0–7, were synthesized. The compounds were studied by static magnetic susceptibility measurements, IR and UV/Vis spectroscopy, and powder X-ray diffraction. The crystal and molecular structures of all compounds were determined by single crystal X-ray diffraction.     

Synthesis,crystal structure,and density functional theory study of a new compound 4-(2-chlorobenzyl)-1-(5-fluoro-2-hydroxy-3-(thiomorpholinomethyl)phenyl [1,2,4]triazolo[4,3-a]quinazolin-5(4H)-one

In this paper, a novel SHP244 derivative 4-(2-chlorobenzyl)-1- (5-fluoro-2-hydroxy-3- [thiomorph-olinomethyl] phenyl)- [1,2,4]triazolo [4,3-a] quinazolin-5(4H)-one was synthesized through five steps. The single crystals were grown in a suitable solvent system (dichloromethane and methanol). Its structure was confirmed by ¹H NMR, ¹³C NMR spectroscopy, ESI-MS, m/z: 534.12[M-H] (MS), FT-IR, and X-ray single crystal diffraction. The crystal structure of the title compound was optimized by density functional theory (DFT) calculation. The crystal structure after X-ray single crystal diffraction was compared with the structure optimized by DFT calculation, and the result shows that the two structures are consistent. In order to explore certain physical and chemical properties, the frontier molecular orbital and molecular electrostatic potential of the title compound were analyzed. In addition, the docking of the title compound to the target protein was studied to understand the docking effect of the compound with the target protein.