Synthesis and X-ray structure of [H3O+·18-crown-6] [Br−Br−Br−]; a compound containing both H3O+ and a linear and symmetrical Br 3 t- ion crystallized from aromatic solution

[H₃O⁺·18-crown-6][Br–Br–Br^–] crystallizes in the triclinic space group P 1 witha=6.105(1),b=8.658(1),c=11.072(1)Å, =71.35(1), =77.58(1), =71.09(1)⁰, andD _c=1.68 g cm^–3 forZ=1. Refinement based on 1112 observed reflections led toR=0.044. The cation exhibits a planar oxonium ion bonded symmetrically to the 18-crown-6 (O(oxonium) resides 0.092 Å out of the plane of the crown ether oxygen atoms). The anion also resides on a center of inversion with Br–Br=2.530(1)Å.     

Hydrothermal crystallization and X-ray structure determination of a new decavanadate with mixed cations [Mn(H2O)6]2[N(CH3)4]2[V10O28]·2H2O

A new decavanadate with mixed cations, [Mn(H₂O)₆]₂[N(CH₃)₄]₂[V₁₀O₂₈]·2H₂O (1), was crystallized from a hydrothermal reaction between MnCO₃ and V₂O₅ in the presence of N(CH₃)₄Br at 100°C. The structure of 1, as determined by x-ray single crystal analysis, consists of cations and anions of hexa-aqua manganese [Mn(H₂O)₆]²⁺, tetramethyl ammonium [N(CH₃)₄]⁺ and decavanadate [V₁₀O₂₈]^6–. The extended H-bonding between the [Mn(H₂O)₆]²⁺ and [V₁₀O₂₈]^6– ions gives rise to a pseudo- two-dimensional network in the crystal lattice x-ray crystallographic data for 1: monoclinic P2₁/n, a = 9.1499(5), b = 12.8725(7), c = 18.625(1) Å, = 92.252(1)°, V = 2192.0(2) ų, MZ = 2, and D _calcd = 2.22 g cm^–3.     

Air-stable liquid clathrates. 1. Crystal structure of [NBu4][Br3] and reactivity of the [NBu4][Br3]·5 C6H6 liquid clathrate

[NBu₄][Br₃] interacts with C₆H₆ to form an air-stable liquid clathrate. The tribromide anion reacts with phenol to give para-bromophenol in>95% yield. The HBr which is generated in the reaction combines with the Br^– anion to form [Br-H-Br]^–. The latter forms the basis for a new liquid clathrate, [NBu₄][Br-H-Br]·n C₆H₆. The parent salt, [NBu₄][Br₃], crystallizes in the monoclinic space group C2/c witha=12.983(5),b=10.380(7),c=16.222(6) Å,=93.93(3)°, andD _c =1.47 g cm^–3 forZ=4. The final R value is 0.068 based on 787 observed reflections.     

KTm[B4O6(OH)4] ⋅ 3H2O: A New Member of Borate Family with Mica-like Tetrahedral Layers

Crystallography Reports - Crystals of new borate KTm[B4O6(OH)4] ? 3H2O (sp. gr. Р $$\bar {3}$$ 1m, a = 4.5472(7) Å, c = 12.151(3) Å) have been obtained under hydrothermal...     

An investigation of the growth of β-BaB2O4 crystals in the BaB2O4-NaF system and new fluoroborate Ba2Na3[B3O6]2F

Crystallography Reports - The phase formation in the BaB2O4-NaF cut has been investigated by the methods of solid-phase synthesis, visual polythermal analysis, and spontaneous crystallization on a...     

Growth, structure, and properties of ferroelectric—ferroelastic— superionic K3Nb3B2O12 and K3−x NaxNb3B2O12 crystals

The potassium niobate-borate K₃Nb₃B₂O₁₂ (KNB) crystals and their solid solutions with partial substitution of potassium by sodium (KNB: Na) are grown from flux and their physical properties are studied. The specific feature of the crystals grown is a complicated polymorphism and the unique combination of ferroelectric and ferroelastic properties with superionic conductivity with respect to potassium ions.     

New framework hydrous silicate K3Sc[Si3O9] · H2O related to the high-temperature anhydrous silicate K3Ho[Si3O9] and symmetry analysis of a phase transition with prediction of structures

Crystals of a new framework silicate K₃Sc[Si₃O₉] · H₂O, space group Pm2₁ n (nonstandard setting of space group Pmn2₁ = C _2v ⁷), are obtained under hydrothermal conditions. The structure is determined without preliminary knowledge of the chemical formula. The absolute configuration is determined. The structure is close to that of the high-temperature K₃Ho[Si₃O₉] phase, which was obtained upon the heating of K₃HoSi₃O₈(OH)₂. This structural similarity is due to the specific conditions of synthesis and an analogous formula, where holmium is replaced by scandium. A symmetry analysis shows that the high local symmetry of a block (rod) is responsible for the first-order phase transition of both the order-disorder (OD) and displacement type. The number of structures in which the simplest and high-symmetry layers are multiplied by different symmetry elements are predicted.     

Structures and properties of layered barium borates Ba0.975[B6O9(OH)(O0.975Br0.025) · B2O(OH)3], Ba2[B5O8(OH)2](OH), Na2Ba2[B20O34(OH)4], and Ba5[B20O33(OH)4]H2O

A new hexaborate, Ba_0.975[B₆O₉(OH)(O_0.975Br_0.025) · B₂O(OH)₃], was synthesized under hydrothermal conditions. This compound is structurally similar to tunnelite and the synthetic borates Pb[B₆O₁₀(OH) · B₂O(OH)₃], Pr[B₆O₁₀(OH) · B₂O(OH)₄], and Nd[B₆O₁₀ · B₃O₃(OH)₄] · H₂O studied earlier. In the new hexaborate and the refined pentaborate Ba₂[B₅O₈(OH)₂]OH, in which the polyanions adopt an orientation in layers unusual for pentaborates, thermal vibrations of the terminal groups were revealed. This fact reflects the real crystal structure. The nonlinear optical properties of the crystals of the polar pentaborate Na₄Ba₄[B₂₀O₃₄(OH)₄] were determined. The crystal structure of the related pentaborate Ba₅[B₂₀O₃₃(OH)₄]H₂O was considered. The factors most likely responsible for the difference in the second-harmonic generation signal for this pair were revealed.     

Crystal and molecular structure of complex compound [Fe3O(CH3COO)6(H2O)3]2[ZnCl4] ⋅ 2H2O

The X-ray crystal structure of trinuclear iron acetate [Fe₃O(CH₃COO)₆(H₂O)₃]₂ [ZnCl₄] ? 2H₂O was determined. The crystal has a ionic structure. It is monoclinic, a = 25.363(7), b = 14.533(4), c = 15.692(4) Å, β = 103.11(2)°, space group _C2/c, and R = 0.0685. The structure of the cationic complex [Fe₃O(CH₃COO)₆(H₂O)₃]⁺ is typical of trinuclear iron(III) compounds containing a μ₃-O bridge: the iron atoms are situated at the vertices of an almost equilateral triangle with the O atom at the center. Each Fe atom is coordinated by four O atoms of bridging carboxy groups, the μ₃-bridging O atom, and the water molecule in the trans position to the latter O atom. Mössbauer spectroscopy evidence indicates the high-spin state (_S = 5/2) of the iron(III) ions.     

Na5[B2P3O13]晶体双晶结构的研究

采用泡生法和b向籽晶生长出尺寸为22mm×24mm×20mm的透明Na5[B2P3O13]晶体.晶体定向中发现(100)和(001)晶面的一级衍射出现双峰;正交偏光显微镜下观察晶体的(010)切片,看到清晰的明暗条纹;当一束激光正入射(010)切片时,产生衍射现象;用同步辐射白光X射线形貌术拍摄了(100)、(010)和(001)切片的Laue像,观察到了晶体的孪晶结构,再借助(010)切片的化学腐蚀研究,推出该晶体为规则的聚片双晶,其结合面为(001).     

Crystal and molecular structure of [H3O·18-crown-6]2-[ReCl6] isolated from a liquid clathrate medium

The crystal and molecular structure of [H₃O·18-crown-6]₂[ReCl₆]1 is reported. Crystal data for1: trigonal, space group R ,a=13.857(2) Å,c=10.154(2) Å,D _c =2.85 g/cm³,Z=3,R _f =0.073,R _w =0.064. The oxonium ion is observed to be crystallographically disordered lying 0.37 Å on both sides of the plane defined by the crown ether oxygen atoms. The anion resides on a crystallographic position forming a slightly distorted octahedron.     

Synthesis, Structure and Properties of (H2NCH2CH2NH3)3 {(VO)6 [B10O16 (OH)6]2} · 11H2O

Abstract A new polyoxovanadoborate cluster (H₂NCH₂CH₂NH₃)₃ {(VO)₆[B₁₀O₁₆(OH)₆]₂} · 11H₂O was prepared by hydrothermal technique and characterized by single crystal X-ray diffraction analysis, IR and TGA. The crystal of the new compound belongs to monoclinic system, space group C2/c with a = 20.198(1) ?, b = 13.4476(8) ?, c = 21.602(1) ?, β = 97.067(1)°, V = 5822.8(5) ?³, Z = 4, D _c = 1.956 g cm⁻³, M = 1714.4, μ = 1.066 mm⁻¹, S = 1.905, R = 0.059, R _w = 0.0966. Index Abstract A new polyoxovanadoborate cluster (H2NCH2CH2NH3)3{(VO)6 [B10O16(OH)6]2} · 11H2O was prepared by hydrothermal technique and characterized by single crystal X-ray diffraction analysis, IR and TGA.      

具有倍频效应的硼酸盐Pb2 [B5O9]Br化合物的合成、晶体生长及其性质研究

利用高温固相反应法合成出Pb2 [B5O9]Br硼酸盐粉末.采用PbO-NaF做复合助熔剂,利用顶部籽晶法获得了3 mm ×3 mm ×1.5 mm的透明单晶,X射线粉末衍射数据显示,该晶体属正交晶系,Pnn2空间群,晶胞参数为a=1.1524(1) nm, b=1.1431(1) nm, c=0.65399(3) nm. 红外光谱测量证实晶体结构中含有BO3-3和BO5-4基团.反射光谱表明Pb2 [B5O9]Br的紫外吸收边在250 nm左右.Pb2 [B5O9]Br粉末倍频效应(SHG)测试表明该化合物具有非线性光学效应,信号强度约等同于β-BaB2O4.     

有机模板硼酸盐[C6N2H18]0.5[B5O6(OH)4]的合成、晶体结构及变温荧光性质

以硼酸和有机胺为原料在水溶液体系中合成了一种有机模板硼酸盐[C6N2H18]0.5[B5O6(OH)4](1a),通过X射线单晶衍射仪对其晶体结构进行了检测.此外,对其进行了元素分析、X射线粉末衍射、红外光谱、热重差热分析及固态荧光光谱等表征.结果表明,该化合物属单斜晶系,空间群为P21/n,晶胞参数为a=0.8593(2) nm,b=1.4015(4) nm,c=1.0293(3) nm,β=104.723(3)°,V=1.1989(6) nm3,Z=4.阴离子基团[B506 (OH)4]-通过强的氢键连接形成具有三种不同形状孔道的新颖三维超分子骨架结构.该化合物在波长为248 nm的激发光下,发射出最大发射波长为375 nm的紫外光.对化合物进行不同温度的热处理后,其荧光性质发生了明显的变化.     

Silicogermanate Ba2K2In2[(Si0.8Ge0.2)6O18] · 2H2O As an Analogue of the Natural Zirconosilicate Kostylevite K4Zr2[Si6O18] · 2H2O

Crystallography Reports - Crystals of new silicogermanate Ba2K2In2[(Si0.8Ge0.2)6O18] · 2H2O were prepared by the hydrothermal synthesis; sp. gr. P21/n, a = 6.5548(6) Å, b = 11.6946(10)...     

新型配位聚合物[Zn(C10H7N2O2)Br]n的溶剂热合成及晶体结构

以咪唑对苯甲酸和溴化锌为原料,以乙醇-水为溶剂,通过溶剂热反应合成了一种新型配位聚合物[Zn(C10H7N2O2)Br]n,并对其进行了元素分析、红外光谱表征和X射线单晶衍射测定.该配位聚合物属单斜晶系,空间群P2(1)/c,a=0.83624(6)nm,b=1.5878(1)nm,c=0.8720(6)nm,β=107.804(1)°,V=1.1024(1)nm3,Z=4,dc=2.003 g/cm3,μ=5.836 mm2,F(000)=648.该晶体通过配位键的连接形成二维网状结构.荧光光谱结果表明,配合物在蓝光区有较强的发射.     

Glass formation and third-order optical nonlinear properties within TeO2–Bi2O3–BaO pseudo-ternary system

Tellurite glasses from TeO₂–Bi₂O₃–BaO pseudo-ternary system were prepared using a conventional melt-quenching method and its glass-forming region was determined. A series of glasses were selected and their third-order optical nonlinearities (TONL) were measured by employing the Z-scan method at a wavelength of 800 nm with femtosecond laser pulses. The results showed that glass former Te⁴⁺ ions exhibited positive influences on the TONL and glass modifiers Ba²⁺ ions behaved similarly; low concentrated Bi³⁺ ions as glass modifiers weakened the nonlinearities, but an excess amount of Bi³⁺ behaved oppositely. FTIR measurements demonstrated that chemical bonds especially Te–O_eq vibrated at a high energy level remarkably promoted the TONL susceptibility χ⁽³⁾, and the glass sample with the highest Bi₂O₃ content exhibited the largest χ⁽³⁾ value which was due to the presence of BiO₃ polyhedra.