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Hydrothermal Synthesis and Structure of a New Two-dimensional zincophosphite: Zn_2(HPO_3)_3·H_2DACH(DACH = 1,2-diaminocyclohexane)

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Chinese Journal of Structural Chemistry 2004年第8期23卷 850-854页

作者： PANJian-Xin ZHENGShou-Tian YANGGuo-Yu StateKeyLaboratoryofStructuralChemistry FujianInstituteofResearchontheStructureofMatter TheChineseAcademyofSciencesFuzhouFujian350002China

A new open-framework zincophosphite, Zn2(HPO3)3H2DACH 1, was hydro- thermally synthesized in the presence of 1,2-diaminocyclohexane (DACH) as structure-directing agent. Its structure was determined by single-crystal X-ray diffraction and further characterized by FTIR, elemental analysis, powder X-ray diffraction and thermogravimetric analysis. Crystal data for 1: Mr = 486.88, monoclinic, space group P21/c with a = 10.2287(11), b = 9.7624(11), c = 16.1686(18) , b = 92.573(2), V = 1612.9(3) 3, Z = 4, Dc = 2.005 g/cm3, F(000) = 984, = 3.314 mm-1 and S = 1.152. The final R = 0.0473 and wR = 0.1121 for 2456 observed reflections with I > 2s(I). The inorganic layer consisting of four- and eight-membered rings is constructed of alternating ZnO4 tetrahedra and HPO3 pseudo pyramids by sharing vertices. The organic template molecules reside in the interlayer region and interact with the inorganic network through H-bonds.

关键词： zincophosphite hydrothermal synthesis crystal structure open-framework

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Synthesis and Structure of a Novel Three-dimensional Organo-zincophosphite with Three Intersecting Channels

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Chinese Journal of Chemistry 2005年第3期23卷 255-260页

作者：陈文斌李牛项寿鹤 InstituteofNewCatalyticMaterialScience CollegeofChemistryNankaiUniversityTianjin300071China

The hydrothermal synthesis and X‐ray single crystal diffraction analysis of a novel three‐dimensional organo‐zincophosphite, [HO(CH 2 ) 2 NH 3 ] 2 ·[Zn 3 (HPO 3 ) 4 ], are described. The framework is built up from strictly alternating vertex‐linked ZnO 4 tetrahedron and HPO 3 pseudo pyramid incorporating ethanolamine (EOA) cations into its channels. The structure is formed through ZnO 4 tetrahedron connecting with two kinds of four‐membered ring chains along different directions. There are three intersecting channels with eight‐membered ring windows along [0 1 0], [0 4 15] and [0 – 4 15], which have not been found in organo‐zincophosphites before. Crystal data: [HO(CH 2 ) 2 NH 3 ] 2 ·[Zn 3 (HPO 3 ) 4 ], M r =640.21, Orthorhombic, Fdd 2, a =2.8528 nm, b =0.8426 nm, c =1.6159 nm, Z =8, V =3.884 nm3, R 1 =0.0219, wR 2 =0.0544.

关键词： zincophosphite hydrothermal synthesis three‐dimensional framework intersecting channels

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New zincophosphite with Infinite One-dimensional [Zn(HPO_3)(H_2PO_3)]~– Chains: Synthesis, Characterizations and Spectral Properties

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Chemical Research in Chinese Universities 2011年第1期27卷 19-22页

作者： WANG Lei LUO Yan-ling WEN Yong-hong LI Guang-hua FENG Shou-hua Key Laboratory of Eco-chemical Engineering Ministry of Education College of Chemistry and Molecular Engineering Qingdao University of Science and Technology Qingdao 266042 P. R. China State Key Laboratory of Inorganic Synthesis and Preparative Chemistry College of Chemistry Jilin University Changchun 130012 P. R. China

With dimethylamine as a template, a new one-dimensional zincophosphite （C2H8N）·[Zn（HPO3）（H2PO3）] was prepared under hydrothermal conditions and characterized by single-crystal X-ray diffraction, FTIR spectrametry, elemental analysis, powder X-ray diffraction, and thermogravimetric analysis. The compound crystallized in the Monoclinic space group P2（1）/c, with cell parameters, a=0.78410（9） nm, b=1.54744（2） nm, c=0.81418（1） nm, β=105.8150（1）°, V=0.95049（2） nm3 and Z=4. The connectivity of the ZnO4 tetrahedron and HPO3 pseudo pyramid resulted in inifinite corner-sharing 4-membered ring chains, which were further linked by the protonated amine molecules to form a 3D structure via hydrogen bonds. To the best of our knowledge, this is the first existence of a zincophosphite with the anionic framework composition of [Zn（HPO3）（H2PO3）]-. The compound exhibits intense photoluminescence at room temperature.

关键词： Hydrothermal synthesis Organically-templated zincophosphite Structural characterization

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Synthesis and Crystal Structure of a Novel zincophosphite Containing Two-dimensional Inorganic-organic Network

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Chinese Journal of Chemistry 2004年第4期22卷 344-347页

作者：杨雅莉李牛项寿鹤 Institute of New Catalytic Material Science College of Chemistry Nankai University

A novel 1,6-hexamethylenediamine-zincophosphite has been synthesized hydrothermally. Its single-crystal structure refinement has shown the zincophosphite with the composition NH3+ (CH2)(6) NH3+ [Zn(HPO3)(2)](2-), M-r = 343.55. It crystallizes in monoclinic, space group C2/c (No.15), a=2.2391 nm, b=0.8695 nm, c=0.7919 nm, beta = 101.062(6)degrees, V= 1.513 nm(3), D-c=1.508 kg/m(3), Z=4, F(000)=712,mu= 1.849 mm(-1), R-1=0.0416, wR(2)=0.1023. This phase exhibits infinite inorganic chains of vertex-linked ZnO4 and HPO3. Via the electrostatic attraction, 1,6-hexainethylenediamine cations and inorganic chains construct a novel interesting two-dimensional inorganic-organic network.

关键词： zincophosphite hydrothermal synthesis two-dimensional network

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