The alkali hypophosphites KH2PO2, RbH2PO2 and CsH2PO2

The structures of the hypophosphites KH₂PO₂ (potassium hypophosphite), RbH₂PO₂ (rubidium hypophosphite) and CsH₂PO₂ (caesium hypophosphite) have been determined by single‐crystal X‐ray diffraction. The structures consist of layers of alkali cations and hypophosphite anions, with the latter bridging four cations within the same layer. The Rb and Cs hypophosphites are isomorphous.     

Crystal Structure and Properties of Acid Salt of Orthoperiodic Acid CsH9I2O12

The acid salt of orthoperiodic acid CsH₉I₂O₁₂crystallizes in the monoclinic system: base-centered unit cell, space group Cc. Unit cell parameters: a=18.473(5) Å, b= 5.439(2) Å, c= 10.481(3) Å, = 99.73°. The crystal structure consists of layers parallel to the yzcrystallographic axis. The layers are formed by the Cs⁺ions, the molecules of orthoperiodic acid IO(OH)₅, and by the IO₂(OH)^– ₄ions and are joined via hydrogen bonds. The studies of proton conductivity of ceramics reveal their transition into a superionic state at temperatures above 40°C.     

Synthesis,Crystal Structure,and Characterization of a New Adduct 3-Ammoniumphenyl Sulfone Dihydrogenphosphate Phosphoric Acid [C12H14N2SO2](H2PO4)2H3PO4

Abstract

A new adduct 3-ammoniumphenyl sulfone dihydrogenphosphate phosphoric acid, [C₁₂H₁₄N₂O₂S](H₂PO₄)₂H₃PO₄, has been synthesized by slow evaporation at room temperature using 3-aminophenyl sulfone as the structure-directing agent. The structure, determined by single-crystal X-ray diffraction at 293 K, can be described as inorganic layers built by H₂PO₄ ^? groups and H₃PO₄ molecules, parallel to the (a, c) planes at y = 0.5, between which molecules of the organic group [C₁₂H₁₄N₂O₂S]²⁺ are inserted. In this atomic arrangement, hydrogen bonds and van der Waals interactions between the different species play an important role in the tri-dimensional network cohesion. Solid-state ¹³C and ³¹P MAS NMR spectroscopies are in agreement with the X-ray structure.

[Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements for the following free supplemental resource: Tables S1 and S2. Figures S1 and S2.]

GRAPHICAL ABSTRACT      

Crystal Structure of Cesium Dihydrotrifluoride,CsH2F3. Refinement of the Crystal Structures of NMe4HF2 and NMe4H2F3

Single crystals of (NMe₄)(HF₂) were obtained during attempted recrystallization of NMe₄F from fluoroolefin. X‐ray diffraction data show that (NMe₄)(HF₂) crystallizes in the orthorhombic space group Pmmn with unit cell dimensions a = 6.535(2), b = 8.688(3), and c = 5.333(2) Å. The symmetric and virtually linear HF₂ anions exhibit a short F···F distance of 2.256(2) Å. The both crystal structures of (NMe₄)(H₂F₃) (orthorhombic, Pbca, a = 8.509(1), b = 11.273(2), and c = 14.880(2) Å) and CsH₂F₃ (orthorhombic, P2₁2₁2₁, a = 7.345(3), b = 9.126(4), and c = 11.444(4) Å) contain dihydrogentrifluoride anions, H₂F₃^?, which have a bent shape and F···F distances of 2.30‐2.34Å.     

Proton conductivity and interphase interaction in CsH2PO4-SrZrO3 composites

Microstructure, transport, and thermal properties of the composites of (1 ? x)CsH₂PO₄/xSrZrO₃ (x = 0.01–0.2) are studied. Introduction of highly dispersed strontium zirconate results in an increase in low-temperature conductivity by 1–3 orders of magnitude as depedent on the composition, leveling, and disappearance of a superionic phase transition in CsH₂PO₄. The methods of differential scanning calorimetry and thermogravimetry were used to show that a significant change in thermodynamic properties of CsH₂PO₄ in composites at x = 0.1–0.2 is observed due to salt amorphization. According to the data of X-ray phase analysis, there is no chemical interaction between the components and no new compounds are formed. An increase in conductivity is caused by salt disordering due to the interphase surface interaction.     

3-氟-6-碘吡嗪-2-羧酸甲酯的合成及晶体结构

以3-氨基吡嗪-2-羧酸为原料，经酯化反应、亲电反应和重氮化反应合成了3-氟-6-碘吡嗪-2-羧酸甲酯（1），总收率62.34%，其结构经¹H NMR、¹³C NMR和MS确证，用X-单晶衍射法测定了化合物的晶体结构。结果表明：1（CCDC: 1986368）属单斜晶系，空间群C2/c，晶胞参数a=17.6566(5) Å, b=4.74850(10) Å，c=19.6368(6) Å，β=95.6540(10)°，V=1638.39(8) ų，Z=8，R_gt(F)=0.0173，wR_ref(F²)=0.0465，F(000)=1056，μ=3.885 mm^-1。      

Synthesis,Crystal Structure and Properties of Li2Cu5(PO4)4

Li₂Cu^II₅(PO₄)₄ has been obtained by various reactions starting from copper or Cu₂O. Crystallization was achieved using I₂ as oxidant and mineralizer. The new orthophosphate crystallizes in space group P$\bar{1}$ , Z = 2, with a = 6.0502(3) Å, b = 9.2359(4) Å, c = 11.4317(5) Å, α = 75.584(2)°, β = 80.260(2)°, γ = 74.178(2)°, at 293 K. Its structure has been determined from X‐ray single‐crystal data and refined to R₁ = 0.022{wR₂ = 0.058 for 4633 unique reflections with F_o > 4σ (F_o)}. From magnetic measurements μ_eff = 1.51 μ_B/Cu and θ_P = –37.4 K have been determined. The Vis/NIR spectrum of aqua‐green Li₂Cu₅(PO₄)₄ shows a single broad band centered around $\bar{1}$ = 12000 cm^–1. Magnetic behavior and spectrum are discussed within the angular overlap model.     

2,2-二苯基-2-羟基乙酸苯胺加合物的合成及其晶体结构

合成了2,2-二苯基-2-羟基乙酸苯胺加合物(1),其结构经UV,IR和X-射线单晶衍射仪表征。1的分子式为C34H31NO6,分子量为549.60,晶体属于三斜晶系,P1空间群,晶胞系数为:a=8.646(16),b=13.357(2),c=14.117(3),α=69.685(3)°,β=77.593(3)°,γ=71.748(3)°,V=1.441 3(5)nm3,Z=2,Dr=1.266 mg.cm-3,F(000)=580,μ(Mo Kα)=0.087 mm-1。结构由直接法解出,最终偏离因子为R1=0.054 6,wR=0.123 3。1通过分子间氢键连接形成超分子化合物。     

ChemInform Abstract: Hydrothermal Synthesis and Crystal Structure of Na3In(PO4)2.

ChemInform is a weekly Abstracting Service, delivering concise information at a glance that was extracted from about 100 leading journals. To access a ChemInform Abstract of an article which was published elsewhere, please select a “Full Text” option. The original article is trackable via the “References” option.     

Crystal Structure of Calciumpolyphosphate, [Ca2(PO3)4]x

β-Calciumpolyphosphate crystallizes in the monoclinic space group P2₁/c, unit cell a = 6.999, b = 7.717, c = 16.944 Å, β = 90.44°. Full matrix refinement with unit weight lead to R = 0.022. The period of the anion chain amounts to 4 tetrahedra, chain direction is x. The cation polyhedra form double chains, also parallel x, in which the polyhedra are linked by common faces and edges.     

Synthesis and Crystal Structure of Rb3AgO2

Rb₃AgO₂ was prepared via the azide/nitrate route. Stoichiometric mixtures of the precursors (Ag₂O, RbN₃ and RbNO₃) were heated in a special regime up to 450 °C and annealed at this temperature for 50 h in silver crucibles. Single crystals have been grown by subsequent annealing of the as prepared powder at 450 °C for 500 h in silver crucibles, which were sealed in glass ampoules under dried Ar. According to the X‐ray analysis of the crystal structure (P2₁2₁2₁, Z = 16, a = 12.800(1), b = 12.848(1), c = 14.329(1)Å, 6566 independent reflections, R(all) = 0.0795, R_w(all) = 0.0218), Rb₃AgO₂ is isostructural with K₃AgO₂. The structure can be derived from the fluorite structure type. Silver is linearly coordinated by oxygen atoms, while Rb has pseudo‐tetrahedral coordination. The crystal under investigation was composed of four twin individuals.     

Synthesis and Crystal Structure of Na2TiO3

The crystal structure of a sodium titanium oxide Na2TiO3 obtained by high temperature solid state reaction method was determined from single-crystal X-ray diffraction study. The compound crystallizes in the monoclinic system, space group C2/c, Mr = 141.88, a = 9.885(1), b = 6.4133(8), c = 5.5048(7) , β = 115.50(3)o, V = 314.99(7) 3, Z = 4, Dc = 2.992 g/cm3, λ = 0.71073 , μ = 27.80 cm–1, F(000) = 272, T = 295 K, R = 0.0189 and wR = 0.0512 for 30 variables and 370 contributing unique reflections. The three-dimensional structure in Na2TiO3 is constructed by the TiO(1)4O(2) and NaO(1)3O(2)2 groups. The titanium atoms are grouped in the form of trigonal bipyramid and arranged along the c axis by sharing the edges. The structure is compared with other structures of related A2BO3 compounds.     

含2,6-萘二甲酸及2,2′-联吡啶的双核钴配合物的合成和晶体结构

溶液法合成了配合物[Co2(NDC)(BIPY)2(H2O)6]·(NDC)(NDC=2,6-萘二甲酸根,BIPY=2,2′-联吡啶),用X-射线单晶衍射分析确定了该配合物的晶体结构。配合物为三斜晶系,P1空间群,a=0.92239(4)nm,b=1.12616(5)nm,c=1.22119(6)nm,α=94.857(3)°,β=111.843(2)°,γ=112.200(3)°,V=1.05205(8)nm3,Z=2,Dc=1.526Mg·m-3。该配合物由[Co2(NDC)(BIPY)2(H2O)6]2+阳离子和1个游离的2,6-萘二甲酸根阴离子组成。Co2+离子与2,6-萘二甲酸根的1个氧原子,2,2′-联吡啶的2个氮原子和3个水的氧原子配位,形成扭曲的八面体构型。2,6-萘二甲酸根的2个羧基分别以单齿方式桥连2个Co2+离子形成双核配合物。配合物中,配位水分子之间,配位水分子和2,6-萘二甲酸根阴离子之间,以及配位水分子和未配位的2,6-萘二甲酸根阴离子之间形成了丰富的O-H…O氢键,进而将双核配合物连接成三维超分子。     

2-甲基-3-硝基苯乙腈的合成及晶体结构

以2-甲基-3-硝基苯甲醛为原料,通过还原、氯代和氰代单元反应合成出2-甲基-3-硝基苯乙腈,经过制备单晶并用X-射线衍射表征其为2-甲基-3-硝基苯乙腈晶体结构,化合物属单斜晶系,空间群为P2_1/C,分子式C_9H_8O_2N_2,Mr=176.18,晶胞参数a=17.26(3)?、b=1.7950(14)?、c=15.746(3)?、b=117.10(3)°、V=1736.3(7)?3,晶胞密度(计算值)为1.348 Mg·m~3、Z=8、R=0.073、wR=0.197。二个分子组成一个不对称的单元,分子间的芳香环形成20.15(7)o的二面角。     

3-羟基克拉霉素和2'-乙酰基-3-氧代克拉霉素的合成与晶体结构

克拉霉素在不同条件下水解,分别生成3-羟基克拉霉素(2)和3-羟基-8,9,10,11-二脱水-9,12-半缩酮克拉霉素(3),用乙酸酐保护2的C(2')-OH得到2'-乙酰基-3-羟基克拉霉素(4),用Ⅳ-氯代琥珀酰亚胺(NCS)氧化4的C(3)-OH合成了2'-乙酰基-3-氧代克拉霉素(5),采用MS,IR,1H NMR,13C NMR等对这些化合物进行了表征.用X射线单晶衍射法测定了化合物2和5的晶体结构,其均属于正交晶系,P212121空间群.化合物2的晶胞参数a=1.3657(3)nm,6=1.4783(3)nm,c=1.6510(3)nm,Z=4,V=3.3332(12)am3,Dc=1.175 g/cm3,F(000)=1288,μ=0.087mm-1;化合物5的晶胞参数a=1.5124(3)nm,b=1.5247(3)nm,c=1.5288(3)nm,Z=4,V=3.5254(12)nm3,Dc=1.187g/cm3,F(000)=1368.0,μ=0.088 mm-1.     

Synthesis,Crystal Structure,and Conductivity Investigation of a New Monophosphate: (2-CH3OC6H4CH2NH 3)H2PO4

Chemical preparation, crystal structure, thermogravimetric and differential analysis, solid state ³¹P MAS NMR characterization, and IR spectroscopic investigations are given for a new organic cation dihydrogenmonophosphate, (2-CH₃OC₆H₄CH₂NH₃)H₂PO₄. This compound is monoclinic C2/c, with unit cell parameters a = 27.740(8), b = 4.827(2), c = 16.435(3) Å, β = 93.79(2)°, V = 2196 (1) ų, Z = 8, and ρ = 1.422 g · cm^?3. The crystal structure has been determined and refined to R = 0.046 (Rw = 0.056), using 1,746 independent reflections with I > 3σ (I). Its atomic arrangement can be described by infinite polyanions [H₂PO₄] _n ^{n ?}, organized in ribbons alternating with organic cations. Strong hydrogen bonds connect the different components. Electrical conductivity measurements show that the [2-CH₃OC₆H₄CH₂NH₃]H₂PO₄ has a low ionic conductivity value at 403 K.