Tl3Al7S12 — ein neues Al-reiches Thioaluminat: Darstellung,Kristallstruktur und Eigenschaften

Tl₃Al₇S₁₂ — a Novel Al-rich Thioaluminate: Preparation, Crystal Structure, and Properties The new ternary phase Tl₃Al₇S₁₂ was prepared from the binary compounds Tl₂S and Al₂S₃ at 700 °C under vacuum. The structure of a yellow plateshaped single crystal was determined at room temperature. The compound crystallizes in the monoclinic polar space group P2₁ (No. 4) with a = 9.040(2), b = 12.381(2), c = 9.569(2) Å and β = 95.91(2)°. The polymeric anionic part of the structure can be described as a puckered layer-like arrangement of cornersharing [AlS₄]-tetrahedra parallel to (001). The aluminium-sulfur layers are connected via single sulfur atoms. The voluminous monovalent thallium atoms bridge the layers of the anionic framework. The mean Al? S bond lengths are 2.227 Å for μ₂-S? Al and 2.298 Å for μ₂-S? Al. In the strongly asymmetric coordination sphere of thallium the Tl? S bond lengths vary from 3.009(9) to 3.907(9) Å and contain four short and two or three longer distances. A rather short Tl…?Tl distance of 3.619(3) Å is observed between two of the three crystallographically independent Tl atoms, so that a weak bonding interaction has to be discussed. Vibrational spectroscopic data for the new phase are reported and discussed.     

Synthesis and Crystal Structure of Er_2Si_2O_7

1INTRODUCTIONThecompoundwithcompositionIRE,O,:ZSiO,(RE~rareEarth)exhibitsex-tensivepolymorphismthatarecharacterizedbyboundariesateuropiumandholmiumalongtheseriesoftrivalentrareearths.Asfarasthestructureisconcerned,typeCisofspecialstabilitybecauseitsrangecanbeextendedbeyondthesmallestrareearthLug toScs tl'z}.Notlongago,wereportedstructureofNd,Si,O,withstructureformAt33.SynthesisandstructureofErZSiZO7withstructureformCarehereinre-ported.2EXPERIMENTAL'ThestartingmaterialsEr,O,…     

Structure and vibrational spectra of dicyclopentadienylzinc. A DFT study

The quantum-chemical DFT calculations of the Cp₂Zn structure confirm the conclusion made earlier from the vibrational spectra that the sandwich structure (⁵-C₅H₅)₂Zn (A) is not energetically favorable and more favorable are the close in energy -structure (⁵-C₅H₅)(¹-C₅H₅)Zn (B) and -structure (¹-C₅H₅)₂Zn (C). The vibrational spectra of structures B and C with the DFT-derived force fields were calculated. A comparison of the calculated spectra of the isolated Cp₂Zn molecules with the experimental data gives no way of deciding between the B and C structures. It is most likely that the molecule is nonrigid and experiences a strong influence from the nearest environment in solution or in the crystalline state.     

Structure and vibrational spectra of mononitroalkanes

Structures and force fields for several mononitroalkane molecules were determined by ab initio quantum-chemical methods. The data obtained were used for calculation of the frequencies and modes of normal vibrations. Potentialities of different methods (RHF, MP2, and B3LYP) and basis sets for estimation of the structures and spectra were studied.     

Synthesis and Structure of a New Polymorph Ba_2CuSi_2O_7

1INTRODUCTIONTheuniqueelectronicpropertiesofcopperoxidesandoxyhalideshaveattractedmuchattentionduetotheirpotentialapplicationsassupercon-ductors,catalysts,luminescentmaterialsandp-typetransparentconductors[1].Inanefforttoexplorenewframeworkstructuresofmixed-metaloxyha-lidessuchasCuAgOCl,wehaveobtainedanewpolymorphofthebariumdicopperdisilicate,b-Ba2CuSi2O7.Inthispaper,wewillreportthesolid-statesynthesisandcrystalstructureofthisnewphaseanddiscussthedifferencesbetweenthestructuresofb-Ba2C…     

Synthesis and Crystal Structure of 9-Pyridyl-1,8-dioxo-2,3,4,5,6,7-hexahydroxanthene

1 INTRODUCTION The Koevenagel condensation catalyzed by bases or Lewis acid has been the subject of many synthetic applications since its discovery[1] although the pre- sence of catalyst is not always indispensable[2]. Mo- reover, the reaction of aromatic aldehyde with 1,3- cyclohexanedione under different conditions afforded different products[3～6]. In continuing efforts for the application of 1,3-cyclohexanedione derivatives to construct new heterocycles with biological activi- ties[7…     

Na2B2Se7, K2B2S7 und K2B2Se7: Drei Perchalkogenoborate mit neuem polymeren Anionengerüst

Na₂B₂Se₇, K₂B₂S₇, and K₂B₂Se₇: Three Perchalcogenoborates with a Novel Polymeric Anion Network Na₂B₂Se₇ (I 2/a; a = 11.863(4) Å, b = 6.703(2) Å, c = 13.811(6) Å, β = 109.41(2)°; Z = 4), K₂B₂S₇ (I 2/a; a = 11.660(2) Å, β = 6.827(1) Å, c = 12.992(3) Å, β = 106.78(3)°; Z = 4), and K₂B₂Se₇ (I 2/a; a = 12.092(4) Å, b = 7.054(2) Å, c = 13.991(5) Å, β = 107.79(3)°; Z = 4) were prepared by reaction of stoichiometric amounts of sodium selenide (potassium sulfide) with boron and sulfur or of potassium selenide and boron diselenide, respectively, at 600°C with subsequent annealing. The crystal structures consist of polymeric anion chains of composition ([B₂S₇]^2?)_n or ([B₂Se₇]^2?)_n formed by spirocyclically connected five-membered B₂S₃ (B₂Se₃) rings and six-membered B₂S₄ (B₂Se₄) rings. The nine-coordinate alkaline metal cations are situated in between.     

Darstellung,spektroskopische Charakterisierung und Kristallstruktur von (CF3)2C(F)OH2+Sb2F11–

Preparation, Spectroscopic Characterization, and Crystal Structure of (CF₃)₂C(F)OH₂⁺Sb₂F₁₁^– Hexafluoroacetone, (CF₃)₂CO, reacts at –78 °C with the superacid HF/SbF₅ under formation of the primary oxonium salt, (CF₃)₂C(F)OH₂⁺Sb₂F₁₁^–, which is characterized by vibrational spectroscopy and NMR spectra. The salt crystallizes in the triclinic space group P1 with a = 817.9(1), b = 989.0(1), c = 1003.8(1) pm and 2 formula units per unit cell.     

Synthesis and Crystal Structure of Borate Oxide Co_3BO_5

1　ＩＮＴＲＯＤＵＣＴＩＯＮＳｏｌｉｄ ｓｔａｔｅｂｏｒａｔｅｓｅｘｈｉｂｉｔａｖａｒｉｅｔｙｏｆｐｈｙｓｉｃａｌａｎｄｃｈｅｍｉｃａｌｆｅａｔｕｒｅｓ,ｒａｎｇｉｎｇｆｒｏｍｎｏｎｌｉｎｅａｒｏｐｔｉｃａｌｐｒｏｐｅｒｔｉｅｓｏｆ β ＢａＢ2 Ｏ4(β ＢＢＯ) [1 ] ｔｏｔｈｅｃａｔａｌｙｔｉｃａｃｔｉｖｉｔｙｏｆＣｕ2 Ａｌ6Ｂ4Ｏ1 7[2 ] ,ｗｈｉｃｈｈａｖｅａｔｔｒａｃｔｅｄｇｒｅａｔａｔｔｅｎｔｉｏｎｏｆｍａｎｙｓｃｉｅｎｔｉｆｉｃｒｅｓｅａｒｃｈｅｒｓ.Ａｓｐａｒｔｏｆｏｕｒｅｆｆｏｒｔｔｏｓｙｎｔ…     

Synthesis and Crystal Structure of Nd_2Si_2O_7 in Low Temperature Form

1INTRoDUCTIONAmongthesilicates,rareearthdisilicatesarespecialbecausetheyshowexten-sivepolymorphism"~".Theconfigurationof(Si,O,)doubletetrahedraisrelativelyrelatedtoperiodicityoftherareearthelectronicstructures,suchasvariationinionicsizeordiscontinuityinchemicalbondingproperties,andalsousefulfordiscussingthedegreeofd-pffbondinginsilicates.SmolinandShepelevhavesynthesizedhightem-peratureformofNd,Si,O,crystallizedinorthorhombicsystem"'.Werecent1yob-tainedlowtemperatureformofNd,Si,O,,which…     

Darstellung und Eigenschaften von Diphthalocyaninaten des Bismuts, [Bi(Pc)2]k (k = 1−, 0, 1+); Kristallstruktur von gemischtvalentem [Bi(Pc)2] · CH2Cl2

Synthesis and Properties of Diphthalocyaninates of Bismuth, [Bi(Pc)₂]^k (k = 1?, 0, 1+); Crystal Structure of mixed-valent [Bi(Pc)₂] · CH₂Cl₂ Blue di(phthalocyaninato(2-))bismuthate(III), [Bi(Pc^2?)₂]^?, is obtained by the reaction of BiO(NO₃) with molten 1,2-dicyanobenzene in the presence of potassium methylate and isolated as tetra-n-butylammonium (ⁿBu₄N)⁺ and bis(triphenylphosphine)iminium (PNP)⁺ salt. Green mixed-valent [Bi(Pc)₂] · CH₂Cl₂ is prepared by anodic oxidation of [Bi(Pc^2?)₂]^?. It crystallizes in the orthorhombic γ modification (Pnma; a = 28.176(5), b = 22.913(3), c = 7.925(1) Å, Z = 4). The Bi^III ion is eightfold coordinated by the N_iso atoms of the slightly distorted Pc ligands in a square antiprismatic manner. The average Bi? N_iso bond distance is 2.467 Å. The complex is paramagnetic (μ_eff = 1.84 μ_B). Oxidation of [Bi(Pc^2?)₂]^? with bromine yields purple, diamagnetic [Bi(Pc^?)₂]Br_x (1.5 ≤ x ≤ 2.5). The redox properties are investigated electrochemically. UV-Vis-NIR, MIR/FIR and resonance Raman spectra of the new bismuth(III) complexes are discussed and compared with those of diphthalocyaninates of the lanthanides.     

Analysis of atomic displacement parameters and molecular motion in crystals. Part 2. X-ray crystal structure of K2Ru(SO4)2 * 6H2O at 160 K and 295 K

Atomic displacement parameters determined from a single-crystal X-ray-diffraction study on K₂Ru(SO₄)₂ * 6H₂O are analyzed in the molecular mean field approximation. The motion of SO₂ ^2– can be described with a rigid-body model, whereas for [Ru(H₂O)₆]²⁺ internal stretching motion and coupling between stretching motion and overall translation are found to be necessary for explaining the observed atomic displacement parameters. Frequencies and force constants of internal motion are not significantly affected by such couplings. K₂Ru(SO₄)₂ * 6H₂O crystallizes in the monoclinic space groupP2₁/c (No. 14), witha = 6.1211(7)Å,b = 12.226(2) Å,c = 8.916(2)Å, = 105.11(1)°,Z = 2 at 160 K anda = 6.1402(7)Å,b = 12.274(2)Å,c = 8.957(1)Å, = 105.25(1)°,Z = 2 at 295 K. The structure was refined to a finalR(F) of 0.017 at 160 K and of 0.019 at 295 K for 1438 and 1299 observed reflections withF ₀ > 6(F₀) and sin / > 0.617 Å^1–.     

Darstellung und Eigenschaften von Phthalocyaninato(2–)indaten(III) mit einzähnigen Acido-Liganden; Kristallstruktur von Tetra(n-butyl)ammonium-cis-difluoro-Phthalocyaninato(2–)indat(III)-Hydrat

Preparation and Properties of Phthalocyaninato(2–)indates(III) with Monodentate Acido Ligands; Crystal Structure of Tetra(n-butyl)ammonium cis -Difluorophthalocyaninato(2–)indate(III) Hydrate Tetra(n-butyl)ammonium cis-diacidophthalocyaninato(2–)indates(III) with the monodentate acido ligands fluoride, chloride, cyanide and formiate are synthezised by the reaction of chlorophthalocyaninatoindium(III) or cis-dihydroxophthalocyaninatoindate(III) with the respective tetra(n-butyl)ammonium salt or ammonium formiate and are characterized by their UV/VIS spectra and their vibrational spectra. The difluoro-complex salt crystallizes as a hydrate ((ⁿBu₄N)^cis[In(F)₂pc^2–] · H₂O) in the monoclinic space group P2₁/n (no. 14) with cell parameters: a = 13.081(3) Å, b = 13.936(2) Å, c = 23.972(2) Å; β = 97.79(1)°, Z = 4. Hexa-coordinated indium is surrounded by four isoindole nitrogen atoms (N_iso) and two cis-positioned fluorine atoms. The average In–F and In–N_iso distance are 2.0685(4) and 2.2033(5) Å, respectively, and the F–In–F angle is 81.5(1)°. The In atom is displaced outside the centre (Ct) of the N_iso plane towards the fluoride ligands: d(In–Ct) = 0.953(1) Å. The phthalocyaninato(2–) core is nonplanar (unsymmetrical concave distortion).     

Synthesis and Crystal Structure of Ho4S3Si2O7

1 INTRODUCTION Halide fluxes are excellent media for growing single crystals of chalcogenides[1~5]. On our research in the Ln-Cu-Zn-Se system to find new phases and to search for potential infrared ceramic materials, two new compounds, KHo2CuSe4 and KEr2CuSe4, were synthesized from the reaction of the precursor with KCl flux[6]. In an attempt to synthesize the homologous sulfide by the same method using KBr as flux in a sealed evacuated quartz tube, single crystals of Ho4S3Si2O7 w…     

Synthesis, Crystal Structure and Properties of a Novel Tetranuclear Nickel（II） Complex with Azo-enolic-2-hydroxybenzamide

A novel tetranuclear nickel(Ⅱ) complex [Ni4L2(DMF)2(H2O)2·2DMF] (1,H4L=azo-enolic-2-hydroxybenzamide, DMF=N,N-dimethyl-formamide) has been synthesized and characterized by elemental analysis, UV, IR and X-ray single-crystal diffraction characterization. Complex 1 crystallizes in the monoclinic system, space group P21/n with a=8.8944(11), b=14.4583(18), c=18.097(2) , β=90.00(2)o, Z=2 , V=2327.2(5)3 , C40H48N12Ni4O14 , Mr=1155.66, Dc=1.649g/cm 3 , μ=1.672 mm-1 , F(000)=1192, R=0.0392 and wR=0.0958. The local coordination environment around the nickel ions exist a distorted octahedral and quadrangle geometry in the molecular structure. Complex 1 exhibits strong photoluminescent emission in the ultraviolet region at room temperature. The electrochemical studies reveal that redox of Ni 3+ /Ni 2+ in the complex is a quasi-reversible process.     

Synthese und Eigenschaften von Bis(tetra(n-butyl)ammonium)-μ-carbidodi(halogenophthalocyaninato(2–)ferraten(IV)); Kristallstruktur von Bis(tetra(n-butyl)ammonium)-μ-carbidodi(fluorophthalocyaninato(2–)ferrat(IV))-Trihydrat

Synthesis and Properties of Bis(tetra(n-butyl)ammonium)μ-Carbido-di(halophthalocyaninato(2–)ferrates(IV)); Crystal Structure of Bis(tetra(n-butyl)ammonium) μ-Carbido-di(fluorophthalocyaninato(2–)ferrate(IV)) Trihydrate μ-Carbido-di(pyridinephthalocyaninato(2–)iron(IV)) reacts with tetra(n-butyl)ammonium halide (ⁿBu₄N)X) in solution (X = F) or in a melt (X = Cl, Br) to yield bis(tetra(n-butyl)ammonium μ-carbido-di(halophthalo-cyaninato(2–)ferrat(IV)). The fluoro-complex salt crystallizes as a trihydrate monoclinically in the space group P12₁/n1 with the following cell parameters: a = 15.814(1) Å; b = 22.690(5) Å; c = 25.127(3) Å; β = 98.27(1)°, Z = 4. The Fe atoms are almost in the centre (Ct) of the (N_iso)₄ planes (N_iso: isoindoline-N atom) with a Fe–Ct distance of 0.053(1) Å. The average Fe–N_iso distance is 1.939(4) Å, the Fe–(μ-C) distance 1.687(4) Å and the Fe–F distance 2.033(2) Å. The Fe–(μ-C)–Fe core is linear (179.5(3)°). The pc²-ligands are staggered (φ = 42(1)°) with a convex distortion. The asymmetric Fe–(μ-C)–Fe stretch (in cm^–1) is observed in the IR spectra at 917 (X = F), 918 (Cl) and 920 (Br) and the symmetric Fe–(μ-C)–Fe stretch at 476 cm^–1 in the resonance Raman spectra. The IR active asymmetric Fe–X stretch (in cm^–1) absorbs at 336 (X = F), 203 (Cl), 182 (Br), respectively.     

二苄基二氯化锡三苯基氧膦的合成及晶体结构研究

利用二苄基二氯化锡与三苯基氧膦反应 ,合成了目标化合物二苄基二氯化锡三苯基氧膦 ,其结构经元素分析表征。用X 射线单晶衍射测定其晶体结构属于三方晶系 ,空间群为P2 1,a =2 .0 2 7( 4 )nm ,b =0 .9714 ( 17)nm ,c =1.5 5 9( 3)nm ,α =90° ,β =90° ,γ =90° ,Z =4 ,V =3.0 4 9( 10 )nm3 ,Dc =1.4 0 7mg·m-3 ,u =1.0 81mm-1,F( 0 0 0 )=1312 ,R1=0 .0 370 ,wR2 =0 .0 6 88,晶体中心的Sn原子为五配位的畸变三角双锥构型     

Synthesis,Crystal Structure,Vibrational Spectroscopy,and Thermal Behavior of Y[B_2O_3（OH）]_3

The hydroxy yttrium hexaborate,Y[B2O3(OH)]3,has been synthesized under mild hydrothermal conditions at 458 K.The crystal structure was solved and refined from single-crystal X-ray diffraction.It adopts a trigonal space group R3c(No.161) with a = 8.3942(4),c = 20.6484(12) ,V = 1260.03(12) 3,YB6H3O12,Mr = 348.79,Z = 6,Dc = 2.758 g/cm3,F(000) = 1008,μ = 7.015 mm-1,R = 0.0321 and wR = 0.0772.Its crystal structure is made up of six-membered rings,alternating three-connected [BO3(OH)] tetrahedra and planar [BO3] trigonal groups,which are interconnected with each other by sharing their common oxygen corners to form a three-dimensional framework structure with six-membered ring channels that are occupied by the yttrium atoms and run along the c axis.FT-IR,Raman,and TG-DTA results are also presented.     

Synthesis and Structure of the Double Oxide Pb6Re6O19

Pb₆Re₆O₁₉ oxide has been synthesized in a sealed evacuted silica tube and by high-pressure high-temperature technique. Its crystal structure, refined from X-ray powder data (a = 9.3162(1) Å, space group Pn3, R_I = 0.021, R_p = 0.067), is based on a three-dimensional network of Re₂O₁₀ groups linked together by corner sharing. The short Re–Re separation inside the Re₂O₁₀ groups (2.45 Å) indicates the presence of a metal-metal bonding.     

Über die Kristallstruktur von (C6H5)3SiSH und (C6H5)3SiSBr und die Darstellung des Iodsulfans (C6H5)3SiSI

The Crystal Structure of (C₆H₅)₃SiSH and (C₆H₅)₃SiSBr and the Preparation of the Iodosulfane (C₆H₅)₃SiSI The preparation of the halogenosulfanes Ph₃SiSBr and Ph₃SiSI from Ph₃SiSH and N-halogenosuccinimide is reported. They are characterized by vibrational spectroscopic measurements. Ph₃SiSBr crystallizes in space group P1 with a = 899.3(8) pm, b = 941.3(7) pm, c = 1 051.4(7) pm, α = 109.88(5)°, β = 99.23(6)°, γ = 96.78(6)° and Z = 2. Ph₃SiSH crystallizes in space group P2₁/c with a = 1 879.4(8), b = 966.3(5), c = 1 845.2(9), β = 107.84(4), Z = 8. The halogenosulfanes decompose in polar solvents by formation of sulphur and triphenylsilanhalide.