Synthesis and Structure of New Crystal Modification of Tetraphenylantimony 4-Methylbenzenesulfonate

Tetraphenylantimony arenesulfonates were synthesized by the reaction of pentaphenylantimony with arenesulfonyl chlorides in toluene taken in a molar ratio of 1 : 1 : 2 in air. The structure of tetraphenylantimony 4-methylbenzenesulfonate was determined by X-ray diffraction analysis. The Sb atom has a distorted trigonal-bipyramidal coordination with phenyl and arenesulfonate groups in the axial positions. The Sb–C(Ph)_eq bond lengths vary in the 2.099(2)–2.123(2) Å range, and the Sb–C(41) and Sb–O(1) distances are 2.136(2) and 2.499(1) Å, respectively. The O(1)SbC(4) axial angle is 175.77(5)°.     

Tetraphenylantimony Pentafluorobenzoate and Tetra-p-Tolylantimony Nitrate: Syntheses and Structures

The reactions of pentaarylantimony with antimony derivatives Ar₃SbX₂(Ar = Ph or p-Tol and X = OC(O)C₆F₅or NO₃) afford tetraphenylantimony pentafluorobenzoate (Ph₄SbOC(O)C₆F₅) and tetra-p-tolylantimony nitrate (p-Tol₄SbONO₂). The compounds obtained were structurally characterized by X-ray diffraction analysis. The Sb atom in Ph₄SbOC(O)C₆F₅has a distorted trigonal-bipyramidal environment with an axial perfluorobenzoate group. The trigonal-bipyramidal coordination of antimony in p-Tol₄SbONO₂is strongly distorted, with the O atom of the nitrato group lying in the axial plane.     

Synthesis and Crystal Structure of AgCuVO4

Dark red single crystals of AgCuVO₄ were obtained from hydroxide fluxes in Ag‐containers at 430 °C. According to X‐ray diffraction data AgCuVO₄ crystallizes in the orthorhombic space group Pnma (Z = 4, a = 925.5(1) pm, b = 677.8(1) pm, c = 540.1(1) pm, wR2 = 0.0753). The Pearson code (oP28) and Wyckoff sequence (dc⁴a) indicate that AgCuVO₄ is related to the olivine‐type of structure, but the first coordination sphere of Ag^I and Cu^II differ significantly from the C.N. 6 with irregular square‐pyramidal [AgO₅] polyhedra and distorted square‐planar [CuO₄] units. These differences in crystal chemistry are discussed and MAPLE as well as ECoN values are given.     

Synthesis and Structure of 4—Nitrobenzaldehyde Thiosemicarbazone

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NH4ZnPO4的非水合成与晶体结构

从非水体系中制得ＮＨ４ＺｎＰＯ４单晶，并用Ｘ线测定了晶体结构；晶体属六方晶系，Ｐ６３空间群，晶胞参数；ａ＝１．０６８８（２）ｎｍ，ｃ＝８７０６（２）ｎｍ，Ｚ＝８，Ｄｃ＝２．７５１ｇ．ｃｍ＾－３，结构中的锌和磷均为四面体本位，且严格交替排列，无Ｚｎ－Ｏ－Ｚｎ和Ｐ－Ｏ－Ｐ联结方式。     

Synthesis and Modulated Crystal Structure of KBaNbS4

Single crystals of KBaNbS₄ have been prepared by the reaction of Nb with an in situ formed melt of K₂S₃, BaS, and S at 500 °C. Satellite reflections observed in X‐ray diffraction experiments of these crystals indicate the presence of a one‐dimensional lattice distortion. The modulated structure has been solved and refined from X‐ray data using the superspace group approach. KBaNbS₄ can be described in the (3 + 1)‐dimensional superspace group Pnma(α00)0s0 with lattice parameters a = 9.187(1), b = 7.001(1), and c = 12.494(1) Å and a modulation vector q = (0, 0.629(1), 0). In the structure the NbS₄ tetrahedra are stacked along the a axis and show a slight tilting against each other. The K⁺ and Ba²⁺ ions follow this tilting, both are slightly shifted from their positions in the average structure. The modulation does not lead to a significant change in the coordination spheres of the metal atoms. The small effects of the modulation correspond to the relatively weak intensities of the satellite reflections. Results of temperature dependent X‐ray investigations indicate that K⁺ librates at higher temperatures and the surrounding S^2? anions follow this motion. With decreasing temperature the libration of K⁺ is reduced and the coordination geometry freezes under formation of an incommensurate modulation. The heavier Ba and Nb atoms are also affected by positional modulation of the substructure and accommodate to their environment.     

Synthesis and Structure of 4-Trifluoromethylsulfonamidotrichloroethyl-5-chloropyrazoles

Reactions of trifluoromethanesulfonic acid N-(2,2,2-trichloroethylidene)amide with 1,3-dialkyl-5-chloropyrazoles and 1-phenyl-3-methylpyrazole afforded 4-(amidotrichloroethyl)-substituted pyrazole derivatives. 4-Chloropyrazoles were not involved into this process. The structure of compounds synthesized was studied by means of IR and NMR spectroscopy. The presence of intra- and intermolecular hydrogen bonds was revealed by a decrease in the absorption frequencies and a complicated form of ν(NH) and ν_as(SO₂) absorption bands in the IR spectra, and also in splitting of signals in ¹H and ¹³C NMR spectra.__________Translated from Zhurnal Organicheskoi Khimii, Vol. 41, No. 5, 2005, pp. 749–752.Original Russian Text Copyright © 2005 by Kondrashov, Rozentsveig, Sarapulova, Larina, Levkovskaya, Savosik, Bozhenkov, Mirskova.     

Synthesis and Structure of Ag_3PSe_4

The title compound Ag3PSe4 was synthesized by the reaction of Ag powder,P2Se5 and Se in a molar ratio of 1:1:1 at 500℃ and structurally characterized by X-ray crystallography.The crystal belongs to orthorhombic,space group Pmn21 with cell parameters:a=7.689(4),b=6.660(3),c=6.379(4)A,V=326.7(3)A^3,Z=2,Dc=6.816g/cm^3,Mr=670.42,F(000)=584,μ=31.302mm^-1,R=0.0606,wR=0.1289 and S=1.012,The 3-D structure can be regarded as constructed from the stacking of puckered Ag-P-Se honeycomb-like sheets along the c direction,in which the Ag,P and Se atoms are bonded to each other to form a chair-like six-membered ring,and the rings then build the sheets by sharing edges.     

Synthesis,Structure, and Stability of Cs4ZrO4

The colorless Cs₄ZrO₄ is obtained from the reaction of stoichiometric proportions of Cs, CsO₂, and finely divided ZrO₂ in a sealed Ag container at 400–650°C for several days. Regrinding and re-reaction provide a single phase sample. The compound is monoclinic (P2₁/c, Z = 4, a = 7.172 (1) Å, b = 19.907 (1) Å, c = 7.157 (1) Å, β = 113.1 (1)Å, R = 0.032) and isostructural with Cs₄PbO₄, with isolated ZrO₄^4? tetrahedra (d(Zr–O) = 1.97 Å). The compound decomposes to Cs₂ZrO₃ (a) in the presence of excess oxygen or CsO₂, (b) in high vacuum near 275°C, or (c) in a sealed container at about 730 ± 10°C.     

YVO4:Eu发光材料的合成、结构与荧光性——推荐一个大学综合实验

This comprehensive experiment is recommended for the synthesis, structure and fluorescence properties of YVO₄:Eu photoluminescent materials. The main purpose of this experiment is to introduce the research of fluorescent materials, including the synthesis of materials, structure characterization and fluorescence measurement. Students can master the basic principle and operation of instruments, the method for material synthesis, and luminescence properties of the materials. While mastering the basic theory and the basic experimental skills, the experimental ability and creative consciousness, especially their ability to use knowledge comprehensively, can be cultivated and improved. The distance between teaching and scientific research is shortened.     

ChemInform Abstract: Synthesis,Structure, and Electronic Structure of CsAgGa2Se4.

The new title compound is prepared from a mixture of AgGaSe₂ (obtained from the elements at 900 °C, 2 d) and CsI in the molar ratio 1:2 (silica tube, Ar, 800 °C, 48 h).     

3-叠氮-4-氨基呋咱的合成及其晶体结构

以乙二醛和盐酸羟胺为原料,经加成,闭环和氮化反应制备了新型含能化合物3-叠氮-4-氨基呋咱(AAF),其结构经NMR,IR,X-射线单晶衍射仪及元素分析表征。AAF晶体属单斜晶系,P21/c空间群,晶胞参数为:a=0.5329(16)nm,b=1.0722(3)nm,c=0.8492(2)nm,α=90.00°,β=99.03(2)°,γ=90.00°,V=0.5046(2)nm3,Dc=1.660g.cm-3,Z=4,F(000)=256,μ(MoKα)=0.138mm-1。最终偏离因子R1=0.0768,wR2=0.1983。AAF晶体存在分子间氢键。     

Synthesis and Crystal Structure of 4-Aminoquinolinium Dicitratoborate Monohydrate

4-Aminoquinolinium dicitratoborate monohydrate [(4-NH₂)C₉H₆NH][(C₆H₆O₇)₂B] · H₂O (I) has been synthesized for the first time. Single crystals have been studied by X-ray crystallography. The structural units of crystal I are large complex dicitratoborate anions with a spirane structure, 4-aminoquinolinium cations and crystal water molecules. The crystal packing of I is three-dimensional. Seventeen independent contacts O(N)-H?O and N-H?O,O’ form an intricate system of hydrogen bonds.     

4-溴-5-硝基邻苯二甲腈的合成及晶体结构

以邻苯二甲酸酐为原料,经溴化、脱水、亚胺化、硝化、酰胺化、脱水6步反应合成了一种易调变的酞菁前驱体——4-溴-5-硝基邻苯二甲腈,并测定了其晶体结构。     

对二甲胺基苯甲醛缩2,4-二硝基苯腙的合成和结构

利用对二甲氨基苯甲醛和2,4-二硝基苯肼的缩合反应合成了对二甲氨基苯甲醛缩2,4-二硝基苯腙,利用红外、紫外光谱和元素分析进行了结构表征.利用X射线衍射分析方法测定了晶体结构,结果表明化合物中分子为平面型结构,偏离平面的最大的N(2) 原子距平面0.00351(2) nm;分子内和分子间的氢键使晶胞内的分子沿c轴成锯齿型链,分子间有芳环堆积作用存在.     

Synthesis and Crystal Structure of Chiral 4-Hydroxy-4-butyrolactam Fused Aziridine

A novel compound of chiral 4-hydroxy-4-butyrolactam fused aziridine was synthesized via tandem nucleophilic displacement reaction under mild condition. Its structure was determined by IR, 1H NMR, elemental analysis and X-ray diffraction. The crystal of the new compound is of orthorhombic, space group P212121 with a = 6.4246（6）, b = 13.5081（13）, c = 18.6399（18） A, Mr = 278.39, Z = 4, V = 1617.6（3）A^3, Dc = 1.143 g/cm^3, p（MoKa） = 0.075 mm^-1, F（000） = 608, the final R = 0.0297 and wR = 0.0679.     

Two Modifications of NH4HPO3F: Synthesis and Crystal Structure

The α and β modifications of NH₄HPO₃F were synthesized and characterized with single crystal X‐ray diffraction. The crystal structure of α‐NH₄HPO₃F determined at 180 K is monoclinic, space group P2₁/n, with a = 7.4650(1), b = 15.586(2), c = 7.5785(9) Å, β = 108.769(9)°, V = 834.9(2) ų, Z = 8, and R₁ = 0.0376 and wR₂ = 0.0818. β‐NH₄HPO₃F measured at 310 K crystallizes in the triclinic space group, P 1, with a = 7.481(1), b = 7.511(1), c = 7.782(1) Å, α = 84.31(1), β = 84.20(1), γ = 68.67(2)°, V = 404.31(9) ų, Z = 4, and R₁ = 0.0254 and wR₂ = 0.0735. A phase transition was not observed between 180 and 310 K for β‐NH₄HPO₃F. Both modifications of NH₄HPO₄F consist of HPO₃F^– and NH₄⁺ units. Two pairs of two unique anions are linked to each other by O–H…O hydrogen bonds to form cyclic tetramers held together by N–H…O bonds. No O–H…F or N–H…F bonds were observed.     

Synthesis and Structure of 1-Nitro-4-benzothiazolylsulfanyl- and -sulfonyldienes

1-Nitro-4-benzothiazolylsulfanyl- and -sulfonyldienes were synthesized. The former were obtained by thiylation of 1,4-dinitrodienes, and the latter were prepared from the former by oxidation with hydrogen peroxide. The spatial structure of compounds obtained was considered.     

Synthesis and Crystal Structure Analysis of KAg11(VO4)4

New potassium silver vanadate KAg₁₁(VO₄)₄ was obtained by reacting the stoichiometric mixture of Ag₂O and V₂O₅ at elevated oxygen pressure, adding a small portion of aqueous KOH. The synthesis was done at 573 K and 430 MPa of oxygen pressure. The crystal structure was solved by direct methods basing on single crystal diffraction data (Pbca, Z = 4, a = 16.533(1), b = 10.6286(7), c = 10.5452(7) Å, 3983 independent reflections, R₁ = 5.4 %). The optical band gap for KAg₁₁(VO₄)₄ was determined as 2.0 eV. According to magnetic measurements, KAg₁₁(VO₄)₄ is diamagnetic.