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含乳清酸配体的两个单核配合物的合成与晶体结构(英文)

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无机化学学报 2003年第8期19卷 879-884页

作者：吴阿清蔡丽珍郭光华郑发鲲郭国聪毛江高黄锦顺结构化学国家重点实验室中国科学院福建物质结构研究所福州350002 中国科学院研究生院北京100039

The two complexes [Cu(C5H2N2O4)(H2O)3]·2H2O (1) and [Ni(C5H2N2O4)(H2O)4]·H2O (2) were synthesized by self assembly reactions of Cu(NO3)2·3H2O or Ni(CH3COO)2·4H2O with orotic acid (2,6 dioxo 1,2,3,6 tetrahydro 4 pyrimidinecarboxylic acid), respectively. Their crystal structures were determined by single crystal X ray diffraction analyses. Crystallographic data for complex 1: C5H8N2CuO7·2H2O, Mr=307.7, monoclinic P21/n, a=0.57710(1)nm, b=1.76863(6)nm, c=1.09955(4)nm, β=98.600(2)°, V=1.109.63(6)nm3, Z=4 , Dc=1.842g·cm-3, μ(MoKα)=2.010mm-1, F(000)=628, R=0.0436, wR=0.1015, And for complex 2: C5H10N2NiO8·H2O, Mr=302.88, orthorhombic Pbcn, a=2.0763(1)nm, b=1.69355(9)nm, c=0.73478(4)nm, V=2.5837(2)nm3, Z=8, Dc=1.557g·cm-3, μ(MoKα)=1.538 mm-1, F(000)=1248, R=0.0545, wR=0.1305. The X ray analyses revealed that the Cu? and Ni? atoms are both coordinated by carboxylic O atom and contiguous N atom of the pyrimidine ring. In complex 1 the Cu? atom has a slightly distorted square pyramid coordination environment with additional three water molecules, while in complex 2 the Ni? atom adopts a slightly distorted octahedral geometry with additional four water molecules. The three dimensional frameworks of the two complexes are formed by intermolecular hydrogen bonding interactions. CCDC: 1, 204881; 2, 204882.

关键词：乳清酸配体单核配合物合成晶体结构铜配合物镍配合物

Two Novel Zinc Compounds with in situ Formation of Dimethylamine Ligand

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Chinese Journal of Structural Chemistry 2008年第6期27卷 667-672页

作者：刘玺吴阿清郭国聪 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of MatterThe Chinese Academy of Sciences

The investigation of the supramolecular interactions between the zinc chloride salts and the crown ether in tetrahydrofuran （THF） with the diffusion of in situ formed DMA （DMA = dimethylamine） ligand leads to two novel zinc-DMA compounds, [（H3O）·（18C-6）][ZnCl3（DMA）] 1 and [（HDMA）·（18C-6）][ZnCl3（DMA）] 2 （18C-6 = 18-crown-6）, whose emissions fall into the blue-emission field. Crystal data for compound 1： monoclinic, space group P21/c, a = 8.753（1）, b = 14.538（2）, c = 19.969（3）A, β = 110.121（7）°, V = 2386.2（5）A^3, T = 293（2） K, Z = 4, Mr = 500.14, Dc= 1.392 g/cm^3,μ = 1.395 mm^-1, F（000） = 1048, S = 1.006, R = 0.0611 and wR = 0.1755 for 3676 observed reflections with I 〉 2σ（I） and 235 parameters. For 2： triclinic, space group P1^-, a = 9.2672（4）, b = 11.8778（2）, c = 13.3846（1） A, a = 67.09（1）, β = 75.54（2）, ）,γ = 81.32（2）°, V = 1311.74（6） A^3, T = 293（2） K, Z = 2, Mr = 527.21, Dc = 1.335 g/cm^3,μ = 1.271 mm^-1, F（000） = 556, S = 1.006, R = 0.0393 and wR = 0.1034 for 3839 observed reflections with I〉 2σ（I）.

关键词： zinc compound in situ crystal structure blue-emission

[COH(NH_2)_2]_2[Cu(pic)_2(ClO_4)_2]的合成与晶体结构(英文)

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无机化学学报 2003年第1期19卷 95-98页

作者：郭光华郭国聪周国伟王明盛蔡丽珍吴阿清黄锦顺结构化学国家重点实验室中国科学院福建物质结构研究所中国科学院研究生院北京100039

GThe title compound was synthesized by reaction of Cu(ClO4)2, picolinic acid and carbamide in C2H5OH/CH3CN solution, and characterized by single crystal X ray diffraction. It crystallizes in the orthorhombic system, space group Pbcawith a=14.0481(8), b=9.0130(5), c=18.626(1)?, V=2358.3(2)?3, Z=4, Dx=1.771g·cm-3, μ=1.235mm-1 and F(000)=1276. The final R factor is 0.0440 for 1434 observed reflections. The X ray analysis revealed that the copper?atom iscoordinated by two picolinic ligands in the equatorial plane, while the two oxygen atoms of perchlorate occupy the axial positions of octahedron with lengthened Cu O distances, resulting in a 4+2 elongated octahedral environment. In the compound, there also exist two protonated carbamide cations for charge balance. CCDC: 195354.

关键词： [COH9NH2)2]2[Cu(pic)2(ClO4)2] 合成 2-吡啶羧酸过渡金属 4+2拉长八面体氢键晶体结构

Syntheses and Crystal Structures of Two Novel 1-D Metal Complexes with Dicyanamide:[Zn(pheen)(dca)_2]n and [Cu(quin)_2(dca)_2]n

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Chinese Journal of Structural Chemistry 2004年第10期23卷 1143-1149页

作者：吴阿清郑发鲲蔡丽珍郭国聪黄锦顺 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter The Chinese Academy of Sciences Fuzhou Fujian 350002 ChinaGraduate School The Chinese Academy of Sciences Beijing 100039 China State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter The Chinese Academy of Sciences Fuzhou Fujian 350002 China

The two complexes [Zn(phen)(dca)2]n 1 (phen = 1,10-phenanthroline, dca = di-cyanamide) and [Cu(quin)2(dca)2]n 2 (quin = quinoline) were synthesized by self-assembly reactions of Zn(CH3COO)24H2O with Nadca and phen ligands, and CuCl22H2O with Nadca and quin ligands, respectively. Their crystal structures were determined by single-crystal X-ray diffraction analyses. Crystallographic data for complex 1: (C16H8N8Zn)n, Mr = 377.67, monoclinic, space group P21/c, a = 10.1322(5), b = 11.0218(6), c = 14.1351(6) ? β = 101.077(2), V = 1549.1(1) 3, Z = 4 , Dc = 1.619 g/cm3, (MoKα) = 1.602 mm-1, F(000) = 760, R = 0.0698 and wR = 0.1558; and for complex 2: (C22H14N8Cu)n, Mr = 453.95, orthorhombic, space group Cmc21, a = 16.679(4), b = 9.153(2), c = 12.937(3) ? V = 1975.0(7) 3, Z = 4, Dc = 1.527 g/cm3, (MoKα) = 1.134 mm-1, F(000) = 924, R = 0.0486 and wR = 0.0981. The structures of complexes 1 and 2 consist of infinite zigzag chains, and their metal atoms have slightly distorted square pyramidal coordination environments with two N atoms of phen or quin ligands and three nitrile N atoms of dca ligands. The secondary long ZnN bonds and p-p stacking interactions make the chains into a three-dimensional network in complex 1.

关键词： synthesis crystal structure complex dicyanamide

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农村浅井水质卫生状况调查

福建环境 1992年第5期9卷 13-14页

作者：吴阿清吴庆国

One-dimensional Supramolecular Chain Based on a Dinuclear Terbium(Ⅲ) 4-Cyanobenzoate Complex

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Chinese Journal of Structural Chemistry 2007年第7期26卷 805-810页

作者：李国清李艳邹文强陈其湧吴阿清郑发鲲郭国聪 Chemistry and Life Science School Quanzhou Normal University Quanzhou State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter The Chinese Academy of Sciences

A new dinuclear Tb（Ⅲ） 4-cyanobenzoate complex [Tb2（4-cba）6（phen）2] （4-Hcba = 4-cyanobenzoic acid and phen = 1,10-phenanthroline） 1 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： C72H40N10O12Tb2, Mr=1554.98, triclinic Pi, a = 9.903（3）, b = 11.769（8）, c = 15.078（8）A, a = 111.42（12）, It = 96.37（19）, γ = 101-24（14）°, V= 1572（1）A3, Z= 1, Dc = 1.642 g/cm^3, F（000） = 768 μ = 2.305 mm^-1, the final R = 0.0205 and wR = 0.0543 for 5479 reflections with I 〉 2σ（I）. Structural analysis shows that 1 displays an isolated dinuclear structure. Two eight-coordinated Tb（Ⅲ） ions are bridged by four 4-cba ligands in the syn-syn bidentate coordination mode, and two other 4-cba ligands chelate these two Tb（Ⅲ） ions. The title complex molecules are connected through π-π stacking interactions to generate a one-dimensional supramolecular chain, The characteristic infrared spectra, luminescent properties and thermogravimetric analyses have also been discussed.

关键词： terbium(Ⅲ) complex 4-cyanobenzoic add crystal structure π-π stacking optical spectroscopy

应用本质安全原理加强化学类实验室安全预防管理

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实验室研究与探索 2014年第5期33卷 283-286页

作者：李志华吴阿清陈涛林恩水中科院福建物质结构研究所质量安全处福建福州350002

我国的安全生产管理坚持安全第一、预防为主的方针,强调了预防在安全管理工作中居于主要地位。本文根据近期化学类实验室所发生的事故类型及特点,分析了此类实验室中存在的主要危险有害因素,继而应用本质安全的原理提出了若干管理措施... 详细信息

我国的安全生产管理坚持安全第一、预防为主的方针,强调了预防在安全管理工作中居于主要地位。本文根据近期化学类实验室所发生的事故类型及特点,分析了此类实验室中存在的主要危险有害因素,继而应用本质安全的原理提出了若干管理措施。本质安全理论强调通过减少危险有害因素来加强安全管理,通过加强对危险化学品、化学实验过程和设备三个方面的本质安全管理,来构建和完善化学类实验室安全管理体系,可以更加有效地预防安全事故的发生。

关键词：本质安全化学类实验室预防安全管理

A Silver Complex of 6,7-Dicyanodipyridoquinoxaline:π-Stacking Interactions and Luminescence

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Chinese Journal of Structural Chemistry 2008年第11期27卷 1398-1403页

作者：陈慧芬李艳王明盛吴阿清郭国聪黄锦顺 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of MatterThe Chinese Academy of Sciences Graduate School of the Chinese Academy of Sciences

The reaction of 6,7-dicyanodipyridoquinoxaline （DICNQ） with AgNO3 in a 1：1 molar ratio by solution method gave a new complex [Ag（DICNQ）2]NO3 1. Single-crystal X-ray diffraction analysis reveals that the complex crystallizes in the space group Ibca of orthorhombic system with eight formula units in a cell. Crystal data for 1： a = 15.7055（17）, b = 18.411（2）, c = 20.680（2）A, V = 5979.7（11）A3, Z = 8, C32Hl2AgN13O3, Mr = 734.42, Dc = 1.632 g/cm3, μ= 0.734 mm-1, F（000） = 2928, S = 1.023 and T= 293（2） K. The final R = 0.0659 and wR = 0.1927 for 2118 observed reflections with I 〉 2σ（I）, and R = 0.0801 and wR = 0.2196 for all data. The complex builds up a packing structure by π-π stacking interactions and shows a luminescent feature.

关键词： silver complex crystal structure,π-πstacking interactions luminescence

Synthesis, Structure, and Magnetic and Optical Properties of a Novel Chain-like Oxalate-bridging Samarium Complex

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Chinese Journal of Structural Chemistry 2007年第9期26卷 1112-1117页

作者：蔡丽珍郭国聪吴阿清付明来董振超 MATSUSHITA Akiyuki State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter The Chinese Academy of Sciences Hefei National Laboratory for Physical Sciences at Microscale University of Science and Technology of China National Institute for Materials Science 1-2-1 Sengen

A new lanthanide complex [Sm（C2O4）（H2O）5]nCln·2nH2O has been obtained by hydrothermal synthetic method. The crystal belongs to monoclinic, space group P21/n, with a = 7.5438（6）, b = 14.3201（11）, c = 10.8608（9）A, β = 94.565（4）°, V = 1169.55（16）A^3, C2H14ClO11Sm, Mr = 399.93, Z = 4, Dc = 2.271 g/cm^3, μ = 5.290 cm^-1, F（000） = 772, the final R = 0.0271 and wR = 0.0632 for 1880 observed reflections with I 〉 2σ（I）. X-ray crystal analysis reveals that each Sm（III） atom is nine-coordinated by four oxygen atoms from two oxalate ligands and five coordinated water molecules in a distorted tricapped trigonal prism. The chain-like structure of lanthanide oxalate is reported for the first time. The fluorescent property and magnetic behavior of the title compound were investigated. The θ of –14.3（2）° and J of –0.26 cm^-1 indicate antiferromagnetic interaction in the molecule.

关键词： lanthanide luminescent magnetic oxalate structure