Pr3Mo4B6O24(OH)3: High-Pressure/High-Temperature Synthesis of an Acentric Rare Earth Molybdenum Borate

We report on the synthesis of a new praseodymium molybdenum borate under high-pressure/high-temperature conditions. The new compound with the sum formula Pr₃Mo₄B₆O₂₄(OH)₃ crystallizes acentrically in the monoclinic space group Cm displaying a new structure type. The structure was solved via single-crystal structure determination. Additionally, the proposed structural model was confirmed by powder X-ray diffraction, second harmonic generation measurement, and single-crystal infrared and Raman spectroscopic investigation.     

Synthesis and Crystal Structure of a Rubidium Lanthanum Borate Rb3La3(BO3)

The title compound was obtained by the flux method and its structure was determined.It crystallizes in monoelinic,space group P2/c with a=11.0024(17).b=9.2979(14),C=14.500(2)(A),β=110.879(2)°.V=1385.9(4)(A)3,Z=4,Mr=908.38,F(000)=1592,=19.601 mm-1,Dc=4.353 g/cm3,the final R=0.0481 and wR=0.1257 for 2532 observed reflections with I>2σ(I).The Rb3La3(BO3)4 structure Can be viewed as a 3-dimensional scaffold-like framework constructed by La-O polyhedra and BOs groups.Two Rb+ ions locate in a channel along the a direction and the rest one in a cavity.     

Crystal Structure of Lithium Yttrium Borate LiY6O5（BO3）3

1 INTRODUCTION In recent years, more and more attention has been paid to rare-earth borates due to their excellent pro- perties, such as YCa4O(BO3)3(YCOB)[1], YAl3(BO3)4 (YAB)[2] and La2CaB10O19[3] for nonlinear optical materials and self-frequency doubling materials as well as YBO3:Eu for red phosphor materials[4] and Li6M1-xCex(BO3)3 (M = Y, Gd) for neutron detec- tors[5]. In this work, we focus our research interest on LiY6O5(BO3)3 as hosts for VUV (vacuum ultraviolet) l…     

Ba3(BO3)(CO3)F: The First Borate Carbonate Fluoride Synthesized by the High-Temperature Solution Method

In contrast to the well-investigated halogen-containing borates and carbonates, very few halogen-containing borate carbonate compounds have been reported. Specifically, no example of borate carbonate fluoride has been synthesized successfully until now. Herein, the planar π-conjugated units [BO₃]³⁻ and [CO₃]²⁻ and the F⁻ ions are introduced simultaneously into one crystal structure resulting in the first borate carbonate fluoride, Ba₃(BO₃)(CO₃)F, by the high-temperature solution method in the atmosphere. Its structure features a hexagonal channel formed by the [BO₃]³⁻ and [CO₃]²⁻ units with the [F₃Ba₈]¹³⁺ trimers filled in the channel. Various characterizations including single crystal- and powder-XRD, EDX, IR, UV-vis-NIR, and TG-DSC, together with the first principles calculation have been carried out to verify the structure and fully understand the structure–property relationships.     

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,Structure and Thermodynamic Property of a New Lithium Borate: Li4[B8O13(OH)2]·3H2O

A new hydrated lithium borate, Li₄[B₈O₁₃(OH)₂]·3H₂O, has been hydrothermally synthesized and characterized by single crystal X‐ray diffraction, FT‐IR spectroscopy, simultaneous TGA‐DTA and chemical analysis. It crystallizes in the triclinic, space group , a=8.4578(5) Å, b=8.7877(5) Å, c=10.8058(7) Å, α=87.740(3)°, β=71.819(3)°, γ=61.569(3)°, Z=2, V=665.26(7) ų, D_c=2.043 g/cm³. Its crystal structure features polyborate anionic layers with the larger odd 13‐membered boron rings constructed by [B₈O₁₃(OH)₂]^4? FBBs. Through designing the thermochemical cycle, the standard molar enthalpy of formation of this borate was determined to be ?(7953.8±6.6) kJ·mol^?1 by using a heat conduction microcalorimeter.     

Polynitrogen chemistry: preparation and characterization of (N5)2SnF6, N5SnF5, and N5B(CF3)4

Metathetical processes were used to convert N5SbF6 into N5[B(CF3)4] and (N5)2SnF6. The latter salt is especially noteworthy because it contains two N5+ ions per anion, thus demonstrating that salts with touching polynitrogen cations can be prepared. This constitutes an important milestone towards our ultimate goal of synthesizing a stable, ionic nitrogen allotrope. The stepwise decomposition of (N5)2SnF6 yielded N5SnF5. Multinuclear NMR spectra show that in HF the SnF5- ion exists as a mixture of Sn2F(10)(2-) and Sn4F(20)(4-) ions. Attempts to isolate FN5 from the thermolysis of (N5)2SnF6 were unsuccessful, yielding only the expected decomposition products, FN3, N2, trans-N2F2, NF3, and N2.     

N(nPr)4[B5O6(OH)4][B(OH)3]2 and N(nBu)4[B5O6(OH)4][B(OH)3]2: Clathrates with a diamondoid arrangement of hydrogen-bonded pentaborate anions

Single-crystal X-ray structure analyses of N(nPr)₄[B₅O₆(OH)₄][B(OH)₃]₂,1, and N(nBu)₄ [B₅O₆(OH)₄][B(OH)₃]₂,2, reveal that these materials are novel clathrates, the isotypic host structures of which are three-dimensional assemblies of hydrogen-bonded [B₅O₆(OH)₄]^– ionsand B(OH)₃ molecules. The assembly of only the pentaborate anions is a distorted (i.e., along [102] elongated) fourconnected diamond-related network. The N(nPr) ₄ ⁺ and N(nBu) ₄ ⁺ ions are trapped within the complex three-dimensional channel systems of the host frameworks. Both1 and2 crystallize monoclinically with space groupP2₁/c andZ=4. The cell constants are:1:a=13.592(5),b=12.082(2),c=17.355(6) Å, =106.60(2)° (298K);2:a=13.874(3),b=12.585(1),c=17.588(4) Å, =107.04(1)° (238 K). The results obtained by both¹¹B and¹³C MAS NMR spectroscopy are discussed. Thermogravimetric studies under a flowing inert-gas atmosphere suggest that water, stemming from polycondensation of the hydrous borate species, is released from the clathrates at ca. 443 K (1) and 398 K (2) before the decomposition of the organic cations starts at ca. 603 K (1) and 603 K (2).Author for correspondence. Supplementary Data relating to this article are deposited with the British Library as supplementary publication No. SUP 82172 (82 pages).     

Co(en)3[B4O5(OH)4]Cl·3H2O和[Ni(en)3][B5O6(OH)4]2·2H2O的合成、结构以及热力学性质

利用水热法合成了两种过渡金属配合物为模板剂的含水硼酸盐晶体Co(en)3[B4O5(OH)4]Cl·3H2O(1) 和 [Ni(en)3][B5O6(OH)4]2·2H2O (2),并通过元素分析、X射线单晶衍射、红外光谱及热重分析对其进行了表征。化合物1晶体结构的主要特点是在所有组成Co(en)33+, [B4O5(OH)4]2–, Cl– 和 H2O之间通过O–H…O、O–H…Cl、N–H…Cl和N–H…O四种氢键连接形成网状超分子结构。化合物2晶体结构的特点是[B5O6(OH)4]–阴离子通过O–H…O氢键连接形成沿a方向有较大通道的三维超分子骨架,模板剂[Ni(en)3]2+阳离子和结晶水分子填充在通道中。     

A New Sodium Borate: Na[B6O8(OH)3]·6H2O·H3BO3

The structure of [B₆H₉NaO₁₄, H₃BO₃, 6H₂O] was determined by single‐crystal X‐ray diffraction and further analyzed by FTIR spectroscopy and differential thermal/thermogravimetric analysis. The asymmetric unit contains Na–O polyhedra (distorted octahedron), [B₆O₈(OH)₃]^– fundamental building blocks, one free water molecule and one free H₃BO₃ molecule. In the hexaborate anion, three B₃O₃ rings are linked by a common oxygen atom with five trigonal and one tetrahedral boron atoms. The hexaborate group is also linked to the oxygenated environment of the sodium atom by three other six‐membered rings, each of which involve two boron atoms, three oxygen atoms, and sodium as the joint atom.     

Ein neues Kupferzinnboratoxid mit isolierten BO3-Baugruppen: Cu5Sn(BO3)2O4

On a New Copper Tin Borate Oxide with Isolated BO₃ Units: Cu₅Sn(BO₃)₂O₄ Single Crystals of the new compound Cu₅Sn(BO₃)₂O₄ were obtained by a B₂O₃ fluxtechnique. They crystallize in a monoclinic distorted variant of a Ludwigite structure with a partly ordered metal distribution. X-ray investigations on single crystals led to the space group C–P2₁/c (No. 14); a = 6.3526(7); b = 9.502(1); c = 12.100(9) Å; β = 93.30(3)°; Z = 4. All metal-sites are distorted octahedraly coordinated by oxygen-ions. The structure contains BO₃-units and oxygen which is not coordinated to boron.     

Ba4Cr2US9: The First Chalcogenide Analogue of the Perovskite‐related (A3A′BO6)m(A3B3O9)n Family

The compound Ba₄Cr₂US₉, which crystallizes in space group P321, consists of one‐dimensional chains separated by Ba²⁺ cations. Each one‐dimensional chain comprises face‐sharing CrS₆ octahedra and US₆ trigonal prisms in the sequence oct oct tp oct oct tp with the U and Cr centers in a linear chain parallel to [001].     

Ba2[Pd(HS2O7)2(S3O10)2]: A Heteroleptic Polysulfatopalladate

The oxidation of elemental palladium with oleum (65 % SO₃) in the presence of barium carbonate in torch‐sealed glass ampoules at 180 °C leads to yellow single crystals of the heteroleptic palladate Ba₂[Pd(HS₂O₇)₂(S₃O₁₀)₂] (triclinic, P ; Z=1; a=884.18(3), b=927.68(3), c=938.77(4) pm; α=60.473(1), β=80.266(2), γ=87.746(2)°). The crystal structure shows the Pd²⁺ ions in a square‐planar coordination of oxygen atoms of two hydrogendisulfate as well as of two trisulfate anions. The compound is the first example of the rarely seen S₃O₁₀^2? and HS₂O₇^? anions acting as ligands in a complex anion and, moreover, the first heteroleptic polysulfatometallate known so far. The complex formation leads to a stabilization of the trisulfate anion relative to its uncoordinated congener. Ba₂[Pd(HS₂O₇)₂(S₃O₁₀)₂] has been further characterized by vibrational spectroscopy and quantum chemical calculations. Thermal analyses by means of thermogravimetric/differential thermal analysis (TG/DTA) measurements show that the compound decomposes to yield elemental palladium and BaSO₄.