The crystal structure of bisphenoxatelluronium dinitrate,C24H16O9N2Te2

Bisphenoxatelluronium dinitrate is monoelinie, P2₁/c: a = 11.638(4), b = 28.266(8), c = 8.546(3) å, β = 119.73(2)°, z = 4 at t = 22°. All atoms including hydrogen were located. The two ring systems, I and II, are folded along their Te-O axes, 147° and 163°, respectively. The average ring bond distances are: Te-C = 2.091, C-C = 1.377, C-O = 1.370 Å. Each Te is bonded to one NO₃ group, Te1-ON1 = 2.485(5), Te2-ON4 = 2.393(4) Å, and an oxygen bridge connects the ring systems, Te1-OB = 1.966(4), Te2-OB = 2.001(4) Å, Te1-OB-Te2 = 125.0(2)°. The bond distances and angles of the structure are compared to those of related compounds.     

The crystal steueture of phenoxatellurine,C12H8OTe

The crystal structure of phenoxatellurine, C₁₂H₈OTe, was determined by X-ray diffracto-meter methods. The crystals are orthorhorhorhombic, P2₁ 2₁ 2₁, a = 6.036(1), b = 8.160(1), c = 20.717(5) Å at t = 22°. The positions of all atoms, including hydrogen, were found. The central ring is folded along the Te-O axis (138°). Average bond distances are Te-C = 2.098, C-O = 1.397, C-C = 1.382 Å. The phenyl rings are planar with a dihedral angle of 145°; C-Te-C = 89.4(3)°, C-O-C = 121.2(5)°. The structure is compared to those of phenoxathionine and pheuothiazine.     

On the crystal structure of Bi2Te2O7

Bi₂Te₂O₇ is orthothobic, space group Pbcn. The lattice parameters derived from a Guinier powder pattern (Si standard) are: a= 22.794 ± 0.005, b= 5.526 ± 0.001, c= 22.065 ± 0.005Å, z= 16. The structure was solved by analysis of single crystal X-ray data and refined on the basis of neutron powder diffraction data. It is an anion-deficient 4: 1: 4 superstructure of fluorite in which the electron lone-pairs of tellurium are stereochemically active. The structural relationships with fluorite and with Bi₂TeO₅ (and other anion-deficient fluorite-related superstructures) have been shown and discussed.     

(C5H7N2)3(AsMo12O40)·3C5H6N2·2H2O的水热合成、晶体结构及催化性能

采用水热法合成了一种新的3-氨基吡啶砷钼多金属氧酸盐配合物(C5H7N2)3(AsMo12O40)·3C5H6N2·2H2O。 通过单晶X射线衍射、红外光谱、紫外光谱和差热-热重对其进行了表征。 用催化消除丙酮的反应为模式反应,测试了配合物的催化性能。 研究结果表明,标题配合物是由Keggin结构[AsMo12O40]3-杂多阴离子、[C5H7N2]+阳离子、[C5H6N2]分子和结晶水分子组成。 配合物属于单斜晶系,P21/n空间群;晶胞参数a=1.33820(12) nm,b=2.2542(2) nm,c=1.9848(2) nm,β=100.27(3)°,V=5.8912(10) nm3,Z=4,Rgt(F)=0.0590,wRref(F2)=0.1882。 配合物对催化消除丙酮具有较好的的活性,催化实验结果表明,160 ℃下,0.20 g的催化剂可将初始浓度均为1.3 g/m3,流速为4.5 mL/min的丙酮完全消除。     

Synthesis, characterization and studies on the third-order optical non-linearities of novel charge-transfer heteropoly complexes (C8H12N2)5H7PMo12O40 and (C8H12N2)3H3PMo12O40·5H2O

Summary Two novel charge-transfer (CT) heteropoly complexes, (C₈H₁₂N₂)₅H₇PMo₁₂O₄₀ (1) and (C₈H₁₂N₂)₃H₃-PMo₁₂O₄₀·5H₂O (2), prepared by reacting p-Me₂NC₆H₄NH₂ with the four-electron heteropoly blue H₇PMo₁₂O₄₀·12H₂O and heteropoly acid H₃PMo₁₂O₄₀· xH₂O, respectively, were characterized by elemental analysis, and u.v., i.r., XPS and e.s.r. spectroscopies. A sizable electron-transfer interaction occurs within the product molecules and the heteropoly anions retain their Keggin structure. Their third-order optical non-linearity coefficients were measured using the Z-scan technique at a concentration of 4.68 × 10⁻⁶ mol dm⁻³ for (1) and 2.79 × 10⁻⁶ mol dm⁻³ for (2), with I ₀ = 2.38 × 10¹³ w m⁻² and λ = 532nm. The |χ⁽³⁾| for (1) is 2.61 × 10⁻¹⁰ esu and |χ⁽³⁾| for (2) is 1.05 × 10⁻¹⁰ esu.     

Synthesis and crystal structure of a two-dimensional bi-layered supramolecular network compound [Cu2(C7H8N4O)4](ClO4)2 (C7H8N4O=pyridine-3-carbaldehyde semicarbazone)

A two-dimensional bi-layered supramolecular compound [Cu₂(C₇H₈N₄O)₄](ClO₄)₂ has been synthesized by the solvothermal method, and characterized via IR and CHN elemental analysis. The single crystal X-ray data of this compound reveal the complex to be dimeric as a result of terminal –NH₂ group of the semicarbazone moiety bridging, which is relatively rare. On this bi-copper(I) complex, another remarkably structural feature is that each Cu atom adopts an unsymmetrical T-shaped geometry comprised of three N atoms from three pyridine-3-carbaldehyde semicarbazone ligands. The molecules are linked into a two-dimensional bi-layered framework by intermolecular N–H?···?O hydrogen bonds.