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Synthesis, Single-crystal Structure, and Optical and Magnetic Properties of CaEr_2S_4

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Chinese Journal of Structural Chemistry 2007年第8期26卷 973-979页

作者： ZENG Hui-Yi Mattausch Hansjtirgen ZHENG Fa-Kun DONG Zhen-Chao GUO Guo-Cong huang jin-shun State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter The Chinese Academy of Sciences Fuzhou Fujian 350002 China Max Planck Institute for Solid State Research Heisenbergstrasse 1 D-70569 Stuttgart Germany Hefei National Laboratory for Physical Sciences at Microscale University of Science and Technology of China Hefei Anhui 230026 China

Brown needle-like crystals of CaEr2S4 were isolated as the major product from a reaction of elements and binary sulfides by a two-step flux technique. CaEr2S4 crystallizes in the orthorhombic space group Pnma with a=12.845（4）, b=3.862（4）, c=13.001（2）（A）, V=645.0（7）（A）3,Z=4, F（000）=880,μ（MoKα）=27.794 mm^-1, the final R=0.0528 and wR=0.0562 for 1070observed reflections with I 〉 3σ（I）. The CaEr2S4 structure forms a three-dimensional framework that consists of interconnected tetra-octahedral Er4S18 fragments. Ca^2＋cations, in a monocapped trigonal prism geometry, are stuffed in two parallel rows into the one-dimensional channels along the b direction. CaEr2S4 is an infrared-transparent semiconductor with a band gap of 1.81 eV. Magnetic susceptibility measurements over 6～300 K indicate a Curie-Weiss paramagnetic behavior for the phase, with an effective magnetic moment of 9.64（1） μB per Er^3＋ ion.

关键词： rare-earth chalcogenides flux crystal growth crystal structure optical and magnetic properties

Synthesis and Crystal Structure of a New Copper(II) Complex with 4-Cyanobenzoic Acid

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Chinese Journal of Structural Chemistry 2005年第11期24卷 1281-1285页

作者： LI Yan WU A-Qing ZHENG Fa-Kun GUO Guo-Cong LU Can-Zhong huang jin-shun State Key Laboratory of Structural Chemistry Fujian Institute of Research on theStructure of Matter The Chinese Academy of Sciences Fuzhou Fujian 350002 China Graduate School The Chinese Academy of Sciences Beijing 100039 China

A new Cu（Ⅱ） complex [Cu（4-cba）（1,10-phen）（H2O）2]（NO3）（4-Hcba = 4-cyanobenzoic acid） has been synthesized by solvothermal reaction in an ethanol/water mixed solution at 100 ℃ and structurally characterized by single-crystal X-ray diffraction. Crystallographic data： C20H16CuN4O7, Mr= 487.91, triclinic, space group PI, a = 7.8420（2）, b = 9.1070（2）, c = 15.1140（6） A, a = 76.889（9）, β = 81.332（11）, γ = 74.844（ 11）°, V = 1009.89（5） A^3, Z = 2, Dc = 1.605 g/cm^3, F（000） = 498, μ = 1.134 mm^-1, the final R = 0.0379 and wR = 0.0865 for 2977 observed reflections with 1 〉 2σ（Ⅰ）. The Cu（Ⅱ） atom is coordinated by two terminal water molecules, one chelating 1,10-phen molecule and one monodentate 4-cba ligand to form a slightly distorted square pyramid. The title complex molecules are connected through hydrogen bonds and π-π stacking interactions to generate a 2D layered network. The thermogravimetric analysis of the title complex has also been discussed.

关键词： copper(Ⅱ) complex,4-cyanobenzoic acid crystal structure hydrogen bonds,π-π stacking

Solid State Synthesis and Crystal Structure of K_3SI

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Chinese Journal of Structural Chemistry 2006年第2期25卷 159-162页

作者： ZHAO Zhen-Qian LIU Xi CHEN Wen-Tong LI Yan WUA-Qing ZENG Hui-Yi GUO Guo-Cong huang jin-shun State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter The Chinese Academy of Sciences Fuzhou Fujian 350002 China Graduate School of the Chinese Academy of Sciences Beijing 100039 China

A new ternary alkali metal chalcogenide halide, K3SI, has been synthesized by solid state reaction method and structurally characterized by X-ray crystallography. The crystal belongs to hexagonal, space group P63cm with a = 11.699（I ）, c = 5.8279（9） A°, Mr = 276.26, V = 690.8（1 ）A°^ 3, Z = 6, D, = 3.985 g/cm^3, F（000） = 756, μ = 9.913 mm^-1, S = 1.004, R = 0.0719 and wR = 0.2204. The title compound is the first example containing S anion in the ternary alkali metal chalcogenide halides family M3QX （M = alkali metal, Q = chalcogenide, X - halide）, which crystallizes in the hexagonal anti-perovskite structure type.

关键词： crystal structure solid state synthesis ternary alkali metal chalcogenide halide

Determination of alcohol compounds using corona discharge ion mobility spectrometry

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Journal of Environmental Sciences 2007年第6期19卷 751-755页

作者： HAN Hai-yan huang Guo-dong jin shun-ping ZHENG Pei-chao XU Guo-hua LI Jian-quan WANG Hong-mei CHU Yan-nan Laboratory of Environmental Spectroscopy and Key Laboratory of Environmental Optics and Technology Anhui Institute of Optics and Fine Mechanics Chinese Academy of Sciences Hefei 230031 China

Ion mobility spectrometry （IMS） is a very fast, highly sensitive, and inexpensive technique, it permits efficient monitoring of volatile organic compounds like alcohols. In this article, positive ion mobility spectra for six alcohol organic compounds have been systematically studied for the first time using a high-resolution IMS apparatus equipped with a discharge ionization source. Utilizing protonated water cluster ions （H2O）nH^＋ as the reactant ions and clean air as the drift gas, alcohol organic compounds, ethanol, 1- propanol, 2-propanol, 1-butanol, 1-pentanol and 2-octanol, all exhibit product ion characteristic peaks in their respective ion mobility spectrometry, that is a result of proton transfer reactions between the alcohols and reaction ions （H2O）nH^＋. The mixture of these alcohols, including two isomers, has been detected, and the results showed that they could be distinguished effectively in the ion mobility spectrum. The reduced mobility values have been determined, which are in very well agreement with the traditional ^63Ni-IMS experimental values. The exponential dilution method was used to calibrate the alcohol concentrations, and a detection limit available for the alcohols is in order of magnitude of a few ng/L.

关键词： alcohols VOCs ion mobility spectrometry proton transfer reaction

Synthesis and Structural Characterization of a New One-dimensional Infinite Chain of Silver(I) Complex with Triphenylphosphine

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Chinese Journal of Structural Chemistry 2004年第6期23卷 547-550页

作者： LIUBing ZHOUGuo-Wei FUMing-Lai CAILi-Zhen GUOGuo-Cong huangjin-shun StateKeyLaboratoryofStructuralChemistry FujianInstituteofResearchontheStructureofMatterTheChineseAcademyofSciencesFuzhouFujian350002China GraduateSchooloftheChineseAcademyofSciences Beijing100039China

The reaction of triphenylphosphine with AgNO3 yielded an unusual nitrate anion bridging one-dimensional infinite chain [Ag(PPh3)NO3] in which the silver(I) atom is three-coordinated by one P atom of triphenylphosphine and two O atoms of two bridging nitrate anions to form a scalene triangle. The complex [Ag(PPh3)NO3] crystallizes in the monoclinic system, space group P21/c with a = 10.281(2), b = 18.596(5), c = 9.180(2) , = 90.60(1), V = 1755.1(7) 3, Z = 4, Mr = 432.15, Dc = 1.635 g/cm3, F(000) = 864 and = 1.254 mm-1. The final R = 0.0606 and wR = 0.1400 for 2188 observed reflections with I > 2(I) out of 3057 unique ones (Rint = 0.0539). IR and elemental analysis of the complex are characterized.

关键词： silver triphenylphosphine infinite chain organic hybrid crystal structure

A　Novel　Cluster［V2（AgPPh3）6S6O2］·2CH2Cl2　Containinga　Cubane－like　Array　of　Six　Silver　and　Two　Vanadium　Atoms

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Chinese Journal of Structural Chemistry 1996年第2期15卷 102-105页

作者： Zheng Fa-Kun huang jin-shun huang Xiao-Yin Zhang Qian-Er (State Key Laboratory of Structure Chemaxtry,Fujian instuute of Research on the Structure of Matter,Chinese Academy of Scicnces,Fuzhou,350002) State Key Lab. of Struct. Chemistry Fujian Inst. Res. Struct. of Matter Chinese Academy of Sciences Fuzhou 350002

ＡＮｏｖｅｌＣｌｕｓｔｅｒ［Ｖ２（ＡｇＰＰｈ３）６Ｓ６Ｏ２］·２ＣＨ２Ｃｌ２ＣｏｎｔａｉｎｉｎｇａＣｕｂａｎｅ－ｌｉｋｅＡｒｒａｙｏｆＳｉｘＳｉｌｖｅｒａｎｄＴｗｏＶａｎａｄｉｕｍＡｔｏｍｓ￥ＺｈｅｎｇＦａ－Ｋｕｎ；... 详细信息

ＡＮｏｖｅｌＣｌｕｓｔｅｒ［Ｖ２（ＡｇＰＰｈ３）６Ｓ６Ｏ２］·２ＣＨ２Ｃｌ２ＣｏｎｔａｉｎｉｎｇａＣｕｂａｎｅ－ｌｉｋｅＡｒｒａｙｏｆＳｉｘＳｉｌｖｅｒａｎｄＴｗｏＶａｎａｄｉｕｍＡｔｏｍｓ￥ＺｈｅｎｇＦａ－Ｋｕｎ；ＨｕａｎｇＪｉｎ－Ｓｈｕｎ?..

关键词： preparation crystal structure tetrathiovanadate vanadium cluster silver cluster

Synthesis, Magnetic Property and Crystal Structure of a Ytterbium-Copper Mixed Metal Complex:Yb_2Cu_3L_6·6H_2O (L=O(CH_2COO)_2)

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Chinese Journal of Structural Chemistry 1997年第3期16卷 228-232页

作者： MAO Jiang-Gao SONG Ling huang jin-shun(State Key Laboratory of Structural Chemistry, Fujtan Institute of Researchon the Structure of Matter, the Chinese Academy of Sciences, Fuzhou 350002) 中科院福建物质结构所结构化学国家重点实验室福建福州

Reaction of hydrated ytterbium nitrate and copper nitrate with diglycolic acid at pH= 7 produced a new Yb-Cu mixed metal complex, Yb2Cu3L6. 6H2O(L= O(CH2COO)2). Complex Yb2Cu3O36C2H36 (Mr= 1437. 23) crystallized in hexagonalP6/mcc (No. 192) with cell parameters of a= 14. 344 (3), c= 15. 470(7) A,V= 2757(2) A 3; Z= 2; F(000) = 1390; Dcalc.= 1- 731 g/cm3 μ(MoKa) =45. 8 cm-1. The final agreernent factors are R= 0. 077 and Rw = 0.089 for 867 observed reflections with I>3δ(I). It has been characterized by elemental analysis, IR spectrum, magnetic measurement and X-ray crystallography. In the complex, the Yb3+ ion is 9-coordinated tothree ether oxygen and six carboxylate oxygen atoms from three ligands, the copper ionis coordinated to four oxygen atoms from four carboxylate groups of four ligands andtwo water molecules. The Yb3+ ions and the Cu2+ ions are connected by the carboxylate groups of the ligands, thus resulting in the formation of the complicated networkstructure.

关键词： preparation crystal structure magnetic property rare earth copper complex

Synthesis　and　Crystal　Structure　of　Trigadolinium　Bromoorthosilicate，Gd_3Br（SiO_4）_2

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Chinese Journal of Structural Chemistry 1996年第4期15卷 280-283页

作者： Mao Jiang-Gao Zhuang Hong-Hui huang jin-shun(State Key Laboratory of Structural Chemistry, Fujtan Instaute of Research onthe Structure of Marter, Chinese Academy of Sciences, Fuzhou 350002) State Key Lab. of Struct. Chemistry Fujian Inst. Res. Struct. of Matter Chinese Academy of Sciences Fuzhou 350002

Crystals of a new lanthanide orthosilicate, Gd_3Br(SiO_4)_2 (M_r=735.82) were prepared by solid state reaction from the GdOBr/V/NH_4Br system at 900℃. The ammonium bromide served as transport gas. The title compound crystallizes on orthorhombic, space group Imma with a=6.960(3), b=18. 176(6), c=6. 284(2) A ; V=794. 9(5) A￣3; Z=4; D_c=6. 12 g/cm￣3 F(000)=1276; μ(MoKα)=301.63cm￣(-1). A full-matrix least-squares structure factors refined with the 484 observed reflections with I>3. 0σ (I) and anisotropic thermal parameters for the Gd atoms gave R=0.061 and R_w=0. 064 respectively. The gadolinium atoms are in two sites and 8-coordinated as GdO_6Br_2 and GdO_7Br bicapped trigonal prism. The Gd(2) atom is disordered and distributed systematically among two I-lattice related(81) positions, the distance between these positions is 1.599 A. The presence of the bromine atoms causes some long Gd - O bonds. The silicon atoms were extracted from the quartz tube.

关键词： crystal structure synthesis gadolinium bromoorthosilicate

Preparation and Crystal Structure of PrNb5O14

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Chinese Journal of Structural Chemistry 1996年第1期15卷 35-39页

作者： Mao Jiang-Gao Zhuang Hong-Hui huang jin-shun(State Key Laboratory of Structural Chemistry, Fujian institute of Research onthe Structure of Matter, Chinese Academy of Scicnces, Fuzhou 350002) State Key Lab. of Struct. Chemistry Fujian Inst. Res. Struct. of Matter Chinese Academy of Sciences Fuzhou 350002

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ＰｒｅｐａｒａｔｉｏｎａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＰｒＮｂ５Ｏ１４￥ＭａｏＪｉａｎｇ－Ｇａｏ；ＺｈｕａｎｇＨｏｎｇ－Ｈｕｉ；ＨｕａｎｇＪｉｎ－Ｓｈｕｎ(ＳｔａｔｅＫｅｙＬａｂｏｒａｔｏｒｙｏｆＳｔｒｕｃｔｕｒａｌＣｈｅｍｉｓｔｒｙ...

关键词： crystal structure preparation praseodymium niobate