In situ Alkylation of 4,4'-Bipyridine in Hydrothermal Synthesis of an Iodoplumbate Inorganic-organic Hybrid with Fluorescence

A novel 1-D iodoplumbate hybrid,2(Pb3I9)3-·3(C14H18N2)2+ 1,has been hydrothermally synthesized and characterized by IR spectra,TGA and single-crystal X-ray diffraction.Complex 1 crystallizes in monoclinic,space group P21/c,with a=12.057(2),b=14.024(3),c=24.742(5) ,β=90.48(3)°,V=4183.6(14)3,Z=4,R=0.0477 and wR=0.0800.The title compound consists of 1-D chains(Pb3I9)n3n-parallel to the [100] direction and stacks of alkylated 4,4'-bipyridium cations running along the [011] direction.Each anionic chain is surrounded by six arrays of alkylated 4,4'-bipyridium cations through extensive C-H…I atypical hydrogen-bonding interactions to afford an interesting 3-D supramolecular network.Significant fluorescent property of the compound was observed at room temperature.     

Synthesis and Crystal Structure of an Interpentateing 3-D Framework Constructed from Mixed Ligands

A novel organic-inorganic hybrid compound constructed from mixed ligands, Co3（SIP）2（bipy）4（H2O）6·6.5H2O （H3SIP = 5-sulfoisophthalic acid, bipy = 4,4′-bipyridyl）, has been hydrothermally synthesized and characterized by IR, TGA and single-crystal X-ray diffraction. The crystal belongs to orthorhombic, space group P212121 with a = 11.395（2）, b = 19.395（4）, c = 30.675（6） A^°, Mr = 1513.05, V= 6779（2） A^°^3, Dc= 1.482 g/cm^3, F（000） = 3120, μ = 0.873 mm^-1, Z= 4, the final R = 0.0439 and wR = 0.119 for 13421 observed reflections with I〉 2σ（I）. The structure of the compound presents a 3-D framework containing Co-bipy 1-D chain and 2-D bilayer motifs and carboxylate spacers, and the connection of 1-D chain and 2-D bilayer motifs by carboxylate ligand results in the final open framework with twofold interpenetration net. A probe reaction of the oxidation of benzaldehyde with H2O2 using the title compound as catalyst was carded out in a liquid-solid system, showing that the compound has high oxidative catalytic activity to the reaction.     

Synthesis,Crystal Structure and Luminescent Property of a 2-D Hybrid Constructed from [Pb_2I_4] Subunits

A novel organic-inorganic hybrid compound, [Pb2I4（bipy）], （bipy = 4,4′-bipyridine）, was synthesized by self-assembly and its structure was determined by X-ray crystallography method The crystal belongs to the monoclinic system, space group P2 1/c with α = 4.4691（9）, b = 15.385（3）, c = 14.136（3） A, β = 93.75（3）°, V= 969.9（3） A^3, Mr = 1078.16, Dc= 3.692 g/cm^3, F（000） = 916, μ = 23.688 mm^-1, Z = 2, the final R = 0.0395 and wR = 0.0887 for 1557 observed reflections with I 〉 2σ（I）. The title compound presents a two-dimensional layer-like structure constructed from [PbI5N] octahedron and bis-bridging ligand 4,4′-bipyridine. The fluorescence of the title compound is also discussed in this communication.     

中硅耐热铸铁中碳和硫的分析

近年来 ,中硅耐热铸铁应用和发展较为迅速 ,其碳和硫含量对材料的性能及用途影响较大 ,是生产过程中需重点控制和测定的元素[1] 。本文在ＥＭＩ Ａ 5 2 0红外碳硫仪上进行了试验[2 ] ,用纯铁打底 ,钨粒锡粒助熔 ,方法简便快速 ,测定结果满意。1　试验部分1.1　仪器与试剂ＥＭＩ