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Synthesis and Crystal Structural Characterization of a Thiosemicarbazone Derived from 4-Acylpyrazolone

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Chinese Journal of Structural Chemistry 2006年第10期25卷 1233-1237页

作者： LIU Guang-Fei LIU Lang HU Xin JIA Dian-Zeng yu kai-bei Institute of Applied Chemistry Xinjiang University Urumqi 830046 China Chengdu Institute of Organic Chemistry The Chinese Academy of Sciences Chengdu Sichuan 610041 China

The reaction of 4-（p-fluobenzoyl）-2,5-dihydro-3-methyl-1-phenyl pyrazol-5-one with thiosemicarbazide in MeOH followed by recrystallization in EtOH gave rise to yellowish lamellar crystals of 4（p-fluo-a-aminothiocarbonyl hydrazonobenzal）-2,5-dihydro-3-methyl- 1-phenyl pyrazol-5-one 1. It crystallizes in orthorhombic, space group Pbca with a = 18.445（4）, b = 11.987（2）, c = 19.249（4） °A,, V= 4256.1（18）°A^3, Z = 8, Mr = 415.49, Dc= 1.297 g/cm^3, T = 296（2） K, F（000） = 1744,μ（MoKα） = 0.186 cm^-1, R = 0.0521 and wR = 0.1211 for 1661 observed reflections with I 〉 2σ（I）. The compound was structurally characterized by elemental analyses, IR and ^1H NMR. The intermolecular hydrogen bonds are present and a two-dimensional framework is formed by two intermolecular hydrogen bonds in the （001） plane.

关键词： pyrazol-5-one thiosemicarhazide crystal structure synthesis

Synthesis and Crystal Structure of {[Mn(H_2O)_4(3,3'-?azpy)](3, 3'-azpy)_3(PF_6)_2}_n

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Chinese Journal of Structural Chemistry 2002年第3期21卷 292-295页

作者： LI Bao-Long CAO Zheng-Bai WANG Shou-Wu XU Zheng yu kai-bei Department of Chemistry and Chemical Engineering Suzhou UniversitySuzhou 215006China Coordination Chemistry Institute State Key Laboratory of Coordination ChemistryNanjing UniversityNanjing 210093China Chengdu Centre of Analysis and Measurement Academia SinicaChengdu 610041China

The complex {[Mn(H2O)4(3, 3?azpy)](3, 3?azpy)3(PF6)2}n (3, 3?azpy = 3, 3? azobispyridine) has been synthesized and characterized. The crystal (C40H40F12MnN16O4P2, Mr = 1153.76) belongs to the triclinic system, space group P with the following crystallographic parameters: a = 10.761(2), b = 11.040(2), c = 23.365(4) ? a = 85.52(1), b = 82.69(1), g = 70.44(1)? V = 2592.5(8) 3, Dc = 1.478 g/cm3, m(MoKa) = 4.16 cm-1, F(000) = 1174, Z = 2, final R = 0.0493 and wR = 0.1158 for the observed reflections (I > 2.00s(I)). The X-ray analysis revealed that manganese(Ⅱ) cation coordination environment is a distorted octahedral geometry, and the Mn2+ cation is coordinated by four oxygen atoms of water in the equatorial plane, while the two nitrogen atoms of 3, 3?azpy occupy the axial positions. The complex forms a one-dimensional chain structure via 3, 3?azpy bridging ligand.

关键词： crystal structure one-dimensional chain manganese complex azobispyridine

Isolation and Crystal Structure of Trans-2,2',4,4'-tetramethyl-6,6'-dinitro Azobenzene

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Chinese Journal of Structural Chemistry 2004年第9期23卷 1005-1008页

作者： WANG Xiao-Ling YANG Bo-Lun LI Zong-Xiao yuAN Chun-Lan yu kai-bei Environmental and Chemical Engineering Institute Xian Jiaotong UniversityXi'an 710049China Department of Chemistry and Chemical Engineering Baoji College of Arts and SciencesBaoji 721007China Chengdu Institute of Organic Chemistry The Chinese Academy of SciencesChengdu 610041China

Trans-2,2?,4,4?-tetramethyl-6,6?-dinitro azobenzene (C16H16N4O4, Mr = 328.32) was isolated from benzene extract of the leaves of Aconitum sungpanense Hand. Mazz. as a new compound, and characterized by spectral methods and X-ray diffraction analysis. It crystallizes in monoclinic system, space group P21/c with a = 8.544(1), b = 13.997(2), c = 7.161(1) ? ?= 112.97(1), V = 788.4(2) ?, Z = 4, Dc = 1.383 g/cm3, F(000) = 344 and ?MoKa) = 0.102 mm-1. The final R = 0.0395 and wR = 0.1140 for 1913 independent reflections with Rint = 0.0109 and 1329 observed reflections with I > 2s(I). The molecule is composed of two phenyl rings through trans N=N.

关键词： trans-2,2′,4,4′-tetramethyl-6,6′-dinitro azobenzene aconitum sungpanense Hand.Mazz. spectral methods X-ray diffraction analysis

Crystal and Molecular Structure of an Inclusion Complex of p-tert-Butylcalix[6]arene with Toluene

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Chemical Research in Chinese Universities 1999年第1期15卷 3-6页

作者： LU Tong-bu LI Xiao-yan JI Liang-nian HAN Bao-hang LIU yu yu kai-bei Department of Chemistry and Center of Measurement Zhongshan UniversityGuangzhou510275 Department of Chemistry Nankai UniversityTianjin300071 Chengd u Center of Analysis a nd Mea surement Aca demia SinicaChengdu610041

An inclusion complex between p-tert-butylcalixarene and toluene was prepared. It crystallized in the monoclinic system with space group P 2 1/ n , a =1.734 7(2) nm, b =1.903 2(2) nm, c =1.972 9(2) nm , β =94.74(1)°, V =6.491 2(14) nm 3, Z =4. The toluene molecule was included in the macrocycle cavity. The calixanene is of a pinched cone conformation.

关键词： p-tert-Butylcalixarene Toluene Inclusion complex

Synthesis and Crystal Structure of Neodymium Complex with Glycine [Nd(Gly)(H_2O)_7]Cl_3

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Chemical Research in Chinese Universities 1999年第4期15卷 306-310页

作者： LI Jun-ran ZHOU Li-ping JIN Tian-zhu yu kai-bei State Key Laboratory of Rare Earth Materials Chemistry and Application Peking UniversityBeijing 100871P.R.China Chengdu Centre for Analysis and Measurement Academic SinicaChendu 610041P.R.China

The title complex [Nd(Gly)(H 2O) 7]Cl 3 was synthesized and its crystal structure was determined by X ray diffraction to obtain a final R value of 0 026 0 and a wR value of 0 086 8. The crystal is of monoclinic system with a space groug Pm . Every two neodymium ions in the crystal are connected with a carboxyl group to form a polymeric chain molecule. And each neodymium ion is further coordinated with seven oxygen atoms from water molecules. The counter ion(Cl -) is non coordinated to fill up the space between the polymeric chains. So the Nd 3+ cation is nine coordinated and the coordination polyhedron is a trigonotetradecahedron. In addition, there exists the mirror symmetry in the complex.

关键词： Neodymium complex Glycine Crystal structure

STUDY ON REACTION OF (μ_3-CCO_2Et)CO_2M(CO)_8(CpMe)(M=Mo,W) WITH Na_2[Fe(CO)_4].SYNTHESIS OF TWO KINDS OF THE NOVEL CLUSTERS EtO_2CCFeCoM(CO)_8(CpMe)H AND (OCC)FeCoM(CO)_8(CpMe)

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Chinese Chemical Letters 1996年第4期7卷 381-384页

作者： Wu, He Ping Ding, Er Run Yin, yuan Qi Huano, Xiao Ying yu, kai bei Lanzhou Inst. of Chemical Physics Chinese Academy of Sciences Lanzhou 730000 Fuzhou Inst. on Structure of Matter Stn. Key Lab. of Structure Chemistry Fuzhou 350002 Chengdu Ctr. of Anal. and Msrmt. Chinese Academy of Sciences Chengdu 610041

The reactions of dusters (μ3- CCO2Et)Co2M (CO)8(MeCp)[M = Mo(2a),W(2b)], derived from the reaction of (μ3-CCO2Et)Co3(CO)9 with Na[M(CO)3(MeCp)], with Na2[Fe(CO)4] in THF at reflux not only gave the expected metal fragment exchange products (μ3-CCO2Et) FeCoM (CO)6(Me-Cp )H [M=Mo(3a), W(3b)] but also produced the unexpected compounds (μ3-CCO)FeCoM (CO)5(MeCp) [M=MO(4a), W(4b)]. It is suggested that the formation of two kinds of compounds resulted from two competitive reactions of the intermediates [(μ3-CCO2Et) FeCo M(CO)8,(MeCp)] with 11+: the one is the Protonic reaction of the intermediate giving the cluster 3a,b; the another one is the intermolecular nucleophilic substitution reaction of the intermediate under the H+ catalytic action giving the cluster 4a,b.

关键词： CO2M CCO2Et AND CLUSTERS EtO2CCFeCoM ON STUDY OF REACTION WITH OCC Na2 Mo

Synthesis and structure of ethyl (Z)-α-formylamino-β-arylacrylates

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Chinese Journal of Chemistry 1991年第1期9卷 60-67页

作者： HAN Ying-Lin HU Hong-Wen ZHOU Zhong-yuan yu kai-bei Department of Chemistry Nanjing UniversityNanjing 210008 Chengdu Analyses and Test Center Academia SinicaChengdu 610015

Ethyl (Z)-α-formylamino-β-arylacrylates were obtained in good yields by the condensation of ethyl N, N-diformylamino acetate and aromatic aldehydes in the presence of sodium ethoxide in ethanol. The structure of eth... 详细信息

关键词： formylamino Synthesis and structure of ethyl arylacrylates

A Cell Solid Structure of cis-1,3-Cyclohexanedicarboxylic Acid and Its Complex Crystal with 4,4'-Dipyridine

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有机化学 2004年第Z1期24卷 51-52页

作者： GAO,Wei yu,kai-bei ZHU,Jin DENG,Jin-Gen Key Laboratory of Asymmetric Synthesis & Chirotechnology of Sichuan Province and Union Laboratory of Asymmetric Synthesis Chengdu Institute of Organic Chemistry Chinese Academy of Sciences Chengdu 610041

Carboxylic acids are important in crystal engineering because they can form strong and directional O-H…O hydrogen bonds as dimmer and catmer.[1] The dicarboxylic acids (not containing other hydrogen bonding groups) generally form the extended line structure interlinked through dimmer,[2] except that oxalic acid forms both the β-oxalic acid linked by dimmer (finite synthon) and the a-oxalic acid by catmer[3] (infinite synthon). A new molecular packing structure of cis-1,3-cyclohexanedicarboxylic acid (CHDA), which is different from line structure,[4] was gotten (P1/2, Figure 1). The novel structure has dimmer and catmer hydrogen bond pairs in the crystal and the hydrogen bond length of O-H…O is 0.268 nm in catmer and 0.264 nm in dimmer. The bond angles of O=C-O vary from 123.1° to 123.8° in catmer and from 123.1° to 122.0° in dimmer comparing with the ones in line structure.……

关键词： oxalic acid hydrogen bonding crystal engineering molecular packing novel structure hydrogen bonds bond length

A NOVEL SYNTHETIC METHOD FOR THE CLUSTERS FeCo_2(CO)_9- (RCCR)(R=MeO_2C,EtO_2C).X-RAY CRYSTAL STRUCTURE ANALYSESOF THE CLUSTERS FeCo_2(CO)_9(MeO_2CCCCO_2Me) and Co_4(CO)_(10)-(EtO_2CCCCO_2Et)

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Chinese Chemical Letters 1996年第6期7卷 585-588页

作者： Wu, He Ping Yin, yuan Qi yu, kai bei Huang, Xiao Ying Lanzhou Inst. of Chemical Physics Chinese Academy of Sciences Lanzhou 730000 Chengdu Anal. Determination Center Chinese Academy of Sciences Chengdu 610041 Fuzhou Inst. Res. Struct. of Matter Chinese Academy of Sciences State Key Lab. of Struct. Chemistry Fuzhou 350002

A novel synthetic method for the clusters FeCo2(CO)9(RCCR)(R=MeO2C,MeO2C), which isthe reaction of Co4(CO)10(RCCR) with Na2[Fe(CO)4], have been found by studying on tile thermal reactionbetween RCCo3(CO)9 with Na2[Fe(CO)4]. X-ray crystal structural determinations have been made for theclusters FeCo2(CO)9(MeO2CCCCO2Me) and Co4(CO)10(EtO2CCCCO2Et)

关键词： CO FeCo2 RCCR ANALYSES CLUSTERS