Growth and characterisation of potassium cobalt nickel sulfate hexahydrate for UV light filters

A new single crystal for ultraviolet light filter, KCNSH (Potassium Cobalt Nickel Sulfate Hexahydrate) was designed and its crystal structure was studied using X‐ray diffraction in this paper. The empirical of the title compound is K₂Co_0.1Ni_0.9(SO₄)₂.6H₂O with formula weight 437.15. KCNSH crystal belongs to the monoclinic space group P2(1)/c, a=6.1390(3)Å, b=12.1839(6)Å, c=9.0095(4)Å, α=γ=90°, β=105.060(2)°, V=650.74(5)ų, Z=2, Dc=2.231g/cm³. Using the cooling solution method, we have grown a deep green KCNSH crystal with dimension of 12×12×40mm³. The transmission spectrum of KCNSH in the range from UV to near IR wavelengths, its thermal properties, and the relationship between the structure and optical transmission properties are also studied and further discussed in this paper. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal growth and structure of KBi(WO4)2 single crystals

Potassium bismuth tungstate [KBi(WO₄)₂] single crystals have been grown by the top‐seeded solution growth technique. Bulk crystal with dimensions up to several centimeters is obtained for the first time. Several self‐flux systems have been used for the growth from the solution and the experiments using K₂W₂O₇ as a solvent are detailed. Powder and single crystal X‐ray diffraction of this crystal are reported. The structure refinement shows that KBi(WO₄)₂ crystallizes in the monoclinic space group C2/c, with a=10.837(3), b=10.586(3), c=7.622(2)Å, β=130.860(3)°, V=661.4(3)ų, and Z=4. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and characterization of a new langasite‐type single crystal Sr3NbAl1.5Ga1.5Si2O14

Single crystals of Sr₃NbAl_1.5Ga_1.5Si₂O₁₄ (SNAGS) with langasite structure have been successfully grown by Czochralski method. The X‐ray diffraction (XRD) verified that the as‐grown crystal was isostructural with A₃BC₃D₂O₁₄ structure and the lattice parameters were calculated as follows: a = 8.242 Å, c = 5.041 Å, V = 296.6 ų. The piezoelectric coefficient d₁₁ was 5.7pC/N, which was 2.47 times of α‐quartz (d₁₁=2.31pC/N). The electric resistivity was up to 3.04×10⁶ Ωcm at 700 °C for X‐cut sample. In addition, the transmission spectrum of the SNAGS crystal showed that it had a high transmittance (>80%) in the range of 350‐800 nm and exceeded 90% above 520 nm. These results suggest that the SNAGS crystals have potential applications in high‐temperature piezoelectric sensors and optical techniques. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

The Crystal and Molecular Structure of 11,12‐dibromo‐ 7,8—benzo‐1,5‐di(p—tolylsulphonyl)‐1,5‐diazacyclononan

The crystal structure of the title compound, C₂₅H₂₆Br₂N₂O₄S₂ was determined by single crystal X‐ray diffraction technique. The crystals are monoclinic, space group C 2/c, with a=20.7142(2) Å b=11.7910(2) Å, c= 10.6735(3) Å, β=98.549(2)°, V=2577.94(9) ų, Z=4. The structure was solved by direct methods and refined by least‐squares methods to a final R=0.046 for 1866 observed reflections with I>2sigma(I). The title compound, displays disordered geometry around the C1 atom located almost on twofold axis. The nine‐membered heterocylic ring is close to the half‐chair conformation. The dihedral angle between phenyl rings is 34.2(1)°.     

Crystal growth,structure and spectroscopic studies of a novel organic single crystal: L‐lysine p‐nitrophenolate monohydrate (LLNP)

A novel organic crystal, L‐lysine p‐nitrophenolate monohydrate (LLNP) has been grown successfully from an aqueous solution by the slow cooling method. Transparent single crystal of dimensions 22 × 12 × 12 mm³ has been obtained. The single crystal X‐ray diffraction has shown that LLNP belongs to the orthorhombic crystallographic system with space group P2₁2₁2₁. The functional groups and vibrational frequencies of the crystal have been identified using IR and Raman spectra. The proton and carbon configurations have been confirmed through ¹H‐NMR and ¹³C‐NMR spectra analyses. The UV‐Vis‐NIR transmittance spectrum for LLNP crystal has been recorded in the range from 200 to 2500 nm. The second harmonic generation (SHG) intensity of LLNP has been measured by powder SHG method and found to be as 4.2 times as that of KDP. The thermal properties have been studied by using thermo gravimetric (TG) and differential thermal analysis (DTA).     

Growth and crystal structure of the layered compound TlGaSe2

The semiconducting compound TlGaSe₂ was grown by solid state reaction technique. The crystal structure of this material was confirmed by single‐crystal X‐ray diffraction. TlGaSe₂ crystallizes in the monoclinic system with space group C2/c (No. 15), Z = 16 and unit cell parameters a = 10.779(2) Å, b = 10.776(1) Å, c = 15.663(5) Å, β = 99.993(6)°. The structural refinement converged to R(F) = 0.0719, R(F²) = 0.0652 and S = 1.17. The structure consists of a three‐dimensional arrangement of distorted TlSe₈ and GaSe₄ polyhedrons. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Powder second harmonic generation measurement and thermal decomposition mechanisms of a new organometallic compound [(18C6)Li][Cd(SCN)3]

Single crystals of a novel nonlinear optical organometallic compound CLTC, ([(18C6)Li][Cd(SCN)₃]), were grown from aqueous solutions via evaporation technique and characterized by IR spectroscopy, thermal gravimetric analysis and X‐ray single‐crystal diffraction. By X‐ray single‐crystal structural analysis it is revealed that the compound crystallized in a noncentrosymmetric space group Cmc2₁ of orthorhombic system with cell parameter a = 14.767(3) Å, b = 15.454(3) Å, c = 10.644(2) Å, V = 2429.0(8) ų and Z = 4. The thermal stability and thermal decomposition of CLTC crystal were investigated by means of thermogravimetry and differential thermal analysis. The second harmonic generation (SHG) efficiency was measured using the Kurtz and Perry powder technique. It was shown that the value of the SHG efficiency of CLCT powder was about 2 times higher than that of potassium dihydrogen phosphate (KDP). (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and characterization of a PbI2 single crystal used for gamma ray detectors

Lead iodide (PbI₂) is an important material for room temperature radiation detectors. In this paper, we have grown PbI₂ single crystal through a special craft, from which γ‐ray detector has also been fabricated. X‐ray diffraction analysis indicates structure of the grown crystal is 2H with hexagonal space group P3m1. Infrared transmission measurement shows transmission rate of the grown crystal sample (10×10×1mm³) reaches 40% averagely in range of 400∼4000cm^‐1. Ultraviolet absorbing test indicates cut‐off wavelength of the sample is 547.6nm, corresponding band gap of 2.27eV. Room temperature detector fabricated from the grown crystal is sensitive to ²⁴¹Am 59.5KeV γ‐ray. Full width at half maximum (FWHM) of the obtained energy spectrum is 26.7KeV. All the results indicate the PbI₂ crystal grown through the special craft is of good characteristics and can be used for γ‐ray detector. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Structure and spectra character of cobalt nickel sulfate twelvehydrate (CNSH) single crystal

The title compound CoNi(SO₄)₂ · 12H₂O has been prepared and its crystal structure determined by single crystal X‐ray differaction at room temperature. The CNSH crystal structure belongs to the monoclinic space group C2/c,a = 9.966(2) Å, b = 7.2265(14) Å, c = 24.218(5) Å, β = 98.32(3)°, V = 1725.9(6) ų, z = 4, Dc = 2.024 gcm⁻³. The optical transmission character of CNSH crystal in aqueous solution is discontinuous in the range from ultraviolet to near IR wavelengths. The relationship between the structure and the optical transmission property is further discussed. (© 2003 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Vibrational,optical and microhardness studies of trimethoprim DL ‐malate

Trimethoprim malate, an organic crystal, has been synthesized using slow evaporation method from its aqueous solution. Structural, optical and the mechanical properties of the grown crystal have been investigated by various characterization techniques which include FTIR spectra, single crystal XRD, UV‐Vis spectra and Vickers microhardness testing. The structure of the compound predicted by analysing the recorded FTIR spectrum compliments the structure determined using single crystal X‐ray diffraction. Single crystal X‐ray diffraction study reveals that the crystals are monoclinic [P2₁/c, a=12.9850 Å, b=9.3038 Å, c=15.6815 Å and β=111.065°]. The UV‐Vis spectrum exhibits maximum transparency (98%) for a wide range suggesting the suitability of the title compound for optical applications. The optical constants have been calculated and illustrated graphically. Microhardness tests have been performed on the cystal under study and the Vicker hardness number has been calculated. The work hardening coefficient is found to be 2.85 which suggest that the crystal belongs to the family of soft materials. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Structural,thermal, mechanical and z‐scan studies on 4‐nitrophenol single crystals

4‐nitrophenol (4‐NP) single crystals have been grown by using slow evaporation and slow cooling techniques. A single crystal with size in the range of 7x3.4x1.8cm³ has been obtained by slow cooling method. The grown crystals have been subjected to various characterization studies. The powder XRD spectrum of 4‐NP reveals the good crystalline nature of the grown crystal. Single crystal XRD studies show that the crystal belongs to monoclinic system with cell parameters of a=6.09 Å, b=8.79 Å, c=11.61 Å, α=γ=90°, β=103.15°. The resultant FTIR spectrum confirms the various functional groups present in 4‐NP. Thermal analysis has been performed on the material to study the thermal stability of 4‐NP. The grown crystals belong to the category of soft materials as confirmed by Vickers Hardness tests. The optical transmiitance of 4‐NP single crystals has been measured from Vis‐IR spectroscopy study. The nonlinear optical properties have been analyzed by z‐scan technique and 4‐NP is found to be self defocusing because of its negative nonlinear refractive index. (© 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth of Nd:Sr3Ga2Ge4O14 crystals by a modified Bridgman method

Bridgman growth of Nd:SGG (Sr₃Ga₂Ge₄O₁₄) crystals has been investigated for the first time. Pt crucible of ∅︁25mm×250mm with a seed well of ∅︁10mm×80 mm is used, and seed is SGG crystal of ∅︁10mm×50mm grown by Bridgman method in advance. The growth parameters are optimized as the furnace temperature is set to 1450∼1500°C, temperature gradient in the crystal‐melt interface is less than 25 K/cm and growth rate is less than 0.5mm/h. The Nd:SGG crystals with 25mm in diameter and 60mm in length are grown successfully from 1.5 to 8at% Nd³⁺ doped stoichiometric Sr₃Ga₂Ge₄O₁₄ melt. The distribution coefficient and concentration of Nd³⁺ in Nd:SGG crystals are obviously higher than those of Nd:YAG crystal. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure and electrochemical property of one‐dimensional complex: [K(cis‐syn‐cis‐ dicyclohexyl‐18‐crown‐6)]2[Cu(mnt)2]

One metalorganic complex [K(cis‐syn‐cis‐ dicyclohexyl‐18‐crown‐6)]₂[Cu(mnt)₂] (mnt = maleonitriledithiolate) has been obtained by the reaction of dicyclohexyl‐18‐crown‐6 with K₂mnt and CuCl₂·2H₂O. The title complex has been characterized by elementary analysis, FT‐IR, UV‐Vis spectroscopy and x‐ray single crystal diffraction. The title complex crystallizes in the triclinic space group P1 with crystallographic data: a = 10.870(6) Å, b = 11.536(6) Å, c = 12.904(7) Å, α = 101.541(10)°, β = 110.573(9)°, γ = 99.441(9)°, V = 1435.2(13) ų, Z = 1, D_calcd = 1.350 g/cm³, F(000) = 615, R₁ = 0.0641, wR₂ = 0.1475. It displays one‐dimensional chain‐like structure formed by [K(cis‐syn‐cis‐ dicyclohexyl‐18‐crown‐6)]⁺ complex cations and [Cu(mnt)₂]^2‐ complex anions through N‐K‐N interactions. Its electrochemical behavior has also been studied by the cyclic voltammetry. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Structure determination of two asymmetrically substituted oxadiazoles from powder diffraction data

The crystal structures of the 1,3,4 oxadiazole compounds N,N‐dimethyl‐N‐[4‐(1,3,4‐oxadiazol‐2‐yl)phenyl]amine ( 1 ) and 2‐methyl‐5‐phenyl‐1,3,4‐oxadiazole ( 2 ) have been determined. In case of 1 no adequate crystals were available; therefore the structure was solved at room temperature from X‐ray powder diffraction data using the method of simulated annealing. This solution is compared to a second one obtained by applying the molecular replacement method. Subsequent Rietveld refinements combined with the so called two stage method based on the data collected to 1.6 Å resolution yielded an R_wp value of 7.27% for 1 . Compound 1 crystallizes in the orthorhombic space group P2₁2₁2₁ with lattice parameters of a = 7.599(4) Å, b = 6.004(2) Å, c = 21.736(3) Å. The crystal structure of 2 was solved by means of single crystal structure analysis (monoclinic space group P2₁/c, a = 8.010(3) Å, b = 10.783(4) Å, c = 19.234(7) Å, β = 90.794(9)°). (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure of 3‐(3‐nitrophenylhydrazonocarbonyl)‐(1H)‐1,2,4‐triazole

The title compound, C₁₀H₈N₆O₃, was synthesized by the reaction of 3‐(1H)‐1,2,4‐triazole hydrazine with 3‐nitrobenzaldehyde in ethanol. The single crystal structure has been determined by X‐ray analysis. The crystal belongs to monoclinic system, space group p2₁/c with cell constant, a = 8.0214(17) Å, b = 17.334(4) Å, c = 8.9070(18) Å, V= 1179.4(4) ų. An intramolecular N—H...O and N—H…N hydrogen bond are observed between the ‐NH group with O atom of the carbonyl group and the ‐NH group with N atom. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth,structure, and superconducting properties of Bi2Sr2Ca2Cu3O10 and (Bi,Pb)2Sr2Ca2Cu3O10‐y crystals

Large and high‐quality single crystals of both Pb‐free and Pb‐doped high temperature superconducting compounds (Bi_1‐xPb_x)₂Sr₂Ca₂Cu₃O_10‐y (x = 0 and 0.3) were grown by means of a newly developed “Vapour‐Assisted Travelling Floating Zone” technique (VA‐TSFZ). This modified zone‐melting technique was realised in an image furnace and allowed for the first time to grow Pb‐doped crystals by compensating for the Pb losses occurring at high temperature. Crystals up to 3×2×0.1 mm³ were successfully grown. Post‐annealing under high pressure of O₂ (up to 10 MPa at T = 500°C) was undertaken to enhance T_c and improve the homogeneity of the crystals. Structural characterisation was performed by single‐crystal X‐ray diffraction (XRD) and the structure of the 3‐layer Bi‐based superconducting compound was refined for the first time. Structure refinement showed an incommensurate superlattice in the Pb‐free crystals. The space group is orthorhombic, A2aa, with cell parameters a = 27.105(4) Å, b = 5.4133(6) Å and c = 37.009(7) Å. Superconducting studies were carried out by A.C. and D.C. magnetic measurements. Very sharp superconducting transitions were obtained in both kinds of crystals (ΔT_c ≤ 1 K). In optimally doped Pb‐free crystals, critical temperatures up to 111 K were measured. Magnetic critical current densities of 2�10⁵ A/cm² were measured at T = 30 K and μ₀H = 0 T. A weak second peak in the magnetisation loops was observed in the temperature range 40‐50 K above which the vortex lattice becomes entangled. We have measured a portion of the irreversibility line (0.1‐5 Tesla) and fitted the expression for the melting of a vortex glass in a 2D fluctuation regime to the experimental data. Measurements of the lower critical field allowed to obtain the dependence of the penetration depth on temperature: the linear dependence of λ(T) for T < 30 K is consistent with d‐wave superconductivity in Bi‐2223. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Three‐Dimensional Structure Constructed via Hydrogen Bonds and π‐π Stacking Interaction. Crystal Structure of [Cu(AFO)2(H2O)2](ClO4)2.2(AFO).2H2O (AFO = 4,5‐Diazafluoren‐9‐one)

The structure of the title complexes [Cu(AFO)₂(H₂O)₂](ClO₄)₂.2(AFO).2H₂O (AFO = 4,5‐Diazafluoren‐9‐one)has been established by single‐crystal X‐ray diffraction. The complex crystallizes in the triclinic space group P‐1 with cell constants a = 7.659(3) Å, b = 11.066(3) Å, c = 14.203(5) Å, alpha = 75.16(3)°, β = 79.87(3)°, gamma = 85.71(3)°, Z = 1. The structure was solved by direct methods and refined to R₁ = 0.0595 (wR₂ = 0.1164). The X‐ray analysis reveals that a pair of AFO ligands chelate to a Cu(II) atom in an asymmetric fashion with one Cu‐N bond being much longer than the other, the Cu(II) atom is further coordinated by a pair of aqua ligands to form an elongated octahedral geometry. In the crystal of the complex, the mononuclear complex cations [Cu(AFO)₂(H₂O)₂]²⁺, uncoordinated AFO molecules, lattice water molecules and perchlorate anions are assembled into 3‐D structure via hydrogen bonds and π‐π stacking interaction.     

High‐quality LaCoO3 single crystal grown by optical floating zone method and its electromagnetic properties

A LaCoO₃ single crystal with 4 mm in diameter and 30 mm in length has been grown by optical floating zone method. The as‐grown crystal is highly crystalline with the rhombohedral perovskite structure (R3c) and grows parallel to the (121) direction. The room temperature resistivity of the as‐grown crystal is 0.12 Ω·cm and the insulator‐metal transition occurs around 500 K. The coercivity and the remanence of the as‐grown crystal are 5 Oe and 6.61×10^–5 μ_B/f.u. at 5 K, respectively. In 1000 Oe under zero‐field cooling, the magnetic susceptibility of the as‐grown crystal shows an upturn in a Curie tail fashion below 35 K, and appears a wave crest over the interval 55 K≤T≤90 K. In addition, a slope change of 1/χ(T) at about 12 K is observed in 50000 Oe under zero‐field cooling. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

The Crystal and Molecular Structure of tert‐Butoxycarbonyl ‐ α‐aminoisobutyryl ‐ isoleucyl ‐methylester

The crystal structure of the synthetic peptide Boc — Aib — Ile ‐ OMe (C₁₆ H₃ 0 N₂ O₅ ) has been determined from three‐dimensional X — ray diffraction data. The peptide crystallizes in triclinic space group P1 with a = 9.570(9), b = 10.261(7), c = 10.610(2) Å , α = 101.9(0), β = 91.7(0), γ = 98.6(0)° V = 1006.1(12) ų, Z = 2, D_calc = 1.09 Mg m^‐3. The structure was solved by direct methods and refined by full‐matrix least‐squares method to an R value of 0.072 (λ = 1.5418Å). The conformation of Aib residue in molecule A is αL and in molecule B is αR. The Ile residue in molecule A adopts folded conformation, while in molecule B it is in the extended region. The peptide units are trans and show significant deviations from planarity.     

Crystal Growth and Basic Characterisation of the Bismuth Borate Bi2B8O15

Top‐seeded growth of Bi₂B₈O₁₅ from a stoichiometric melt is reported. Crystals have been grown with dimensions of up to 24 × 12 × 5 mm³ . Bi₂B₈O₁₅ shows twin domains at room temperature; their origin was investigated by methods of thermal analysis. The domains were found to result from a sluggish phase transition that occurs in a broad temperature range (ΔT ≈ 20 K) around ∼390 K. Unit cell parameters at room temperature were determined: a = 4.3140(6) Å, b = 22.148(2) Å, c = 6.4695(6) Å, β = 105.46(1)° , possible space group P2₁ (no.4), the non‐centrosymmetry was proved using powder SHG.