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(H_2en)_2[Se_2Mo_5O_(21)]2H_2O的水热合成、晶体结构与光谱研究

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Chinese Journal of Structural Chemistry 2004年第6期23卷 605-611页

作者：连照勋黄长沧张汉辉黄细河杨宏芳化学系和固体材料化学重点实验室

在水热条件下, 以SeO2、V2O5、MoO3、K2CO3、en(乙二胺)作为起始原料, 得到了标题化合物(H2en)2[Se2Mo5O21]2H2O, 利用IR、UV、荧光光谱、单晶-X射线衍射等方法对其进行了表征。结构测定表明, 该化合物属于正交晶系, 空间群: P212121, ... 详细信息

在水热条件下, 以SeO2、V2O5、MoO3、K2CO3、en(乙二胺)作为起始原料, 得到了标题化合物(H2en)2[Se2Mo5O21]2H2O, 利用IR、UV、荧光光谱、单晶-X射线衍射等方法对其进行了表征。结构测定表明, 该化合物属于正交晶系, 空间群: P212121, 化学式: C4H24- Mo5N4O23Se2, 晶胞参数: a = 12.1386(7), b = 17.7118(8), c =11.7092(5) ? V = 2517.4(2) ?, Z = 4, Dc = 2.987 g/cm3, Mr = 1133.89, m = 5.419 mm-1, F(000) = 2144, 最终结构偏离因子R = 0.0285, wR = 0.0400, S = 0.904。该化合物由2个双质子化的en、2个H2O分子以及杂多阴离子[Se2Mo5O21]4-组成。其中,杂多阴离子由5个畸变的MoO6八面体以共边或共顶点形式连接构成一个平面骨架; 2个畸变的SeO3四面体和MoO6八面体以共顶点形式连接, 且位于平面的两侧;质子化的en位于4个[Se2Mo5O21]4-离子围成的四面体空位中, 与杂多阴离子和水分子通过氢键连接成无限三维结构。最后我们用B3LYP方法研究了阴离子簇的电子结构。

关键词：乙二胺硒 Strandberg型杂多化合物水热合成晶体结构钼

Synthesis, Crystal Structure and Antitumor Activity in Vitro of a New Benzoate Binuclear Cupper(Ⅱ ) Complex

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Chinese Journal of Structural Chemistry 2009年第1期28卷 15-18页

作者：康杰黄细河许建华蒋智清黄长沧 Department of Chemistry Fuzhou University College of Pharmacy Fujian Medical University

The title compound, [Cu2（C7H5O2）4（C2H6O）2], was synthesized by the reaction of benzoic acid, copper acetate and ethanol in an aqueous solution. Trypan blue dye exclusion method was used in experiment. X-ray single-crystal analysis has revealed that compound 1 （C32H32Cu2O10） crystallizes in the monoclinic system, space group C2/c, Mr = 703.66, a = 47.340（5）, b = 6.6613（4）, c = 22.028（2）A,β = 113.284（4）°, V = 6380.6（10） A^3, Z = 8, Dc= 1.465 g/cm^3, F（000） = 2896,μ = 1.388 mm^-11, the final R = 0.0515 and wR = 0.1172 for 5712 observed reflections with I 〉 2σ（I）. X-ray crystal structure analysis suggests that compound [CH2（C7H5O2）4（C2H6O）2] has a binuclear structure with two Cu（II） atoms coordinated by four benzoate groups and two ethanol molecules. The crystal packing is stabilized by intermolecular O-H...O hydrogen bonds. The compound inhibits the proliferation of K562 cells （chronic myeloid leukemic cells） significantly and dose-dependently in 48 h, and IC50 of K562 is 17.3μg/mL by trypan blue dye exclusion method.

关键词： binudear cupper(Ⅱ) complex crystal structure benzoate antitumor activity K562

Syntheses, Crystal Structures and Characterization of Two New Cadmium(II) Arsonates

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Chinese Journal of Structural Chemistry 2010年第11期29卷 1724-1730页

作者：刘中乾赵亚峰黄细河李浩宏黄长沧 State Key Laboratory Breeding Base of Photocatalysis Department of Chemistry Fuzhou University

Two cadmium arsonate coordination polymers, Cd（HL1）2 （1, H2L1 = 4-aminophenylarsonatic acid） and Cd（H2L2）2·2H2O （2, H3L2 = 2-（4-arsonphenylamino）acetic acid）, have been synthesized and characterized by IR and single-crystal X-ray diffraction. Crystal data for 1： triclinic, space group P1 with a = 5.7559（12）, b = 7.0903（14）, c = 8.9925（18）, α = 89.04（3）, β = 80.79（3）, γ = 85.09（3）o, Dc = 2.496 g·cm-3, μ = 6.095 mm-1, F（000） = 260, Z = 1, the final R = 0.0574 and wR = 0.1376 for 1489 observed reflections with I 〉 2σ（I）. And those for 2： monoclinic, space group P21/c with a = 4.7595（10）, b = 9.925（2）, c = 22.609（5）, β = 91.81（3）°, Dc = 2.167 g·cm-3, μ = 4.168 mm-1, F（000） = 684, Z = 2, the final R = 0.0335 and wR = 0.0815 for 2340 observed reflections with I 〉 2σ（I）. The structure of 1 shows a two-dimensional layer consisting of inorganic chains of {CdN2（AsO3）2} along the a axis linking with the phenyl groups. These layers are further linked through strong interlayer hydrogen bonding interaction to form a three-dimensional hydrogen bond supramolecular architecture. Compound 2 has inorganic chains of {CdO2（AsO3）2} similar to 1, which connect with four adjacent inorganic chains forming a three-dimensional framework.

关键词： syntheses crystal structure cadmium(II) arsonates

纳米微孔杂多化合物Na[Fe2(O2H3)Mo2O8](Ⅰ)和(NH4)[Fe(MoO4)2](Ⅱ)的结构特征

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功能材料 2004年第Z1期35卷 3347-3348页

作者：孙瑞卿吴小园张汉辉黄长沧黄细河福州大学化学系福建福州350002 中国科学院福建物构所结构化学国家重点实验室福建福州350002

通过采用水热合成法得到了二种具有纳米筛孔的氧簇化合物Na[Fe2(O2H3)Mo2O8](Ⅰ)和(NH4)[Fe(Mo O4)2](Ⅱ).晶体(Ⅰ)属于单斜晶系,空间群为C2/m,晶胞参数为:a=9.5450(17),b=6.4381(9),c=0.76405(12)nm;β=116.128(4),Z=2,R1=0.0219,Rw=0.... 详细信息

关键词：金属氧簇化合物钼酸盐纳米微孔杂化物晶体结构

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锌酞菁-多酸电荷转移复合物的合成和表征

锌酞菁-多酸电荷转移复合物的合成和表征

Hydrothermal Syntheses and Characterizations of Two One-dimensional Molybdenum 1,4-Butylenediphosphonates

中国化学会第26届学术年会晶体工程分会场

作者：秦小焕黄细河黄长沧福州大学化学化工学院福州大学化学化工学院福州大学化学化工学院

＜正＞以Keggin结构的磷钼酸（PMo12）、磷钨酸（PW12）为电子受体,锌酞菁（ZnPc）为电子给体,合成了两种新型电荷转移复合物,采用红外、紫外光谱,热重,元素分析和XRD对产物进行表征。光谱分

关键词：电荷转移杂多酸酞菁

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Chinese Journal of Structural Chemistry 2005年第9期24卷 997-1006页

作者：张慧双傅瑞标张建军吴新涛李亚敏黄细河 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 reaction of Ni（CH3COO）2-4H2O, Na2MoO4·H2O, MoO3, 1,10-phenanthroline and 1,4-butylenediphosphonic acid in distilled water at 180℃ for 72 h produced two new compounds： {[Ni（1,10-phen）3][Ni（1,10-phen）2（Mo6O18）（O3P（CH2）4PO3）]·6H2O}n 1 in 15% yield and {[Ni（1,10-phen）2（H2O）2] [Ni（1,10-phen）2 （H2O）（Mo5O15）（O3P（CH2）4PO3）]·6H2O} n 2 in 47% yield. 1 and 2 both feature {MonO3nO3P（CH2）4PO3}^4-（n=5, 6） 1-D anionic chain, which is further decorated and charge compensated by [Ni（1,10-phen）2]^2＋. 1 contains {Mo6O24P2} cluster constructed of three pairs of face-sharing {MoO6} octahedra linked through corner-sharing interaction. 2 exhibits the characteristic structure based on pentanuclear ring of comer- and edge-sharing {MoO6} octahedra capped by three oxygen atoms of {PO3} on each side. The thermogravimetric analyses and magnetic property of 2 were also studied.

关键词： single crystal 1-D polymers hydrothermal 1,4-butylenediphosphonic acid,organic-inorganic hybrid material polyoxomolybdates

Syntheses, Structures and Photoluminescence of Two New Layered Lanthanide Coordination Polymers with Thiophenedicarboxylic Acid and 1,10-Phenanthroline

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Chinese Journal of Structural Chemistry 2009年第11期28卷 1367-1372页

作者：黄细河黄长沧王金根刘冬生孙瑞卿 State Key Laboratory Breeding Base of Photocatalysis Department of ChemistryFuzhou University Department of Chemistry Jinggangshan University

Two isostructural layered coordination polymers constructed from mixed ligands, [Ln2（tdc）3（phen）2（H2O）2] （Ln = Sm 1, Eu 2, H2tdc = thiophene-2,5-dicarboxylic acid, phen = 1,10-phenanthroline）, have been hydrothermally synthesized and characterized by elemental analysis, IR and single-crystal X-ray diffraction. Crystal data for 1： triclinic, space group P1 with a = 10.546（2）, b = 11.201（2）, c = 18.644（4）A, α = 106.69（3）, β = 91.27（3）, γ = 94.43（3）°, Dc = 1.909 g·cm-3, F（000） = 1180, μ = 2.992 mm^-1, Z = 2, the final R = 0.0300 and wR = 0.0656 for 6968 observed reflections with I 〉 2σ（I）. And those for 2： triclinic, space group P1^- with a = 10.557（2）, b = 11.159（2）, c = 18.588（2） A, α = 106.945（6）, β = 91.255（6）, γ = 94.359（6）°, Dc = 1.927 g·cm^-3, F（000） = 1184, μ = 3.204 mm^-1, Z = 2, the final R = 0.0221 and wR = 0.0459 for 6328 observed reflections with I 〉 2σ（I）. The title complexes show a two-dimensional （2D） square grid structure constructed from paddle-wheel-like [Ln2（CO2）4] dimers and tdc ligands. The 2D layers were further assembled into a 3D supramolecular assembly via O-H…O hydrogen bond. The photoluminescence properties of complexes 1 and 2 were investigated.

关键词： hydrothermal synthesis crystal structure lanthanide photoluminescence

Syntheses, Crystal Structures and Characterization of Layered and Layer-pillared Zinc Arsonates

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Chinese Journal of Structural Chemistry 2012年第9期31卷 1301-1308页

作者：林文钊刘中乾黄细河李浩宏吴舒婷黄长沧 Department of Chemistry Fuzhou University

Two zinc arsonate coordination polymers, Zn（4-apa）·H2O （1, 4-apaH2 = 4-amino- phenylarsonatic acid） and Zn（4-apa）（2）, have been hydrothermally synthesized and characterized by elemental analysis, IR and single-crystal and powder X-ray diffraction. Crystal data for 1： monoclinic, space group C2/c with a = 23.056（5）, b = 5.4224（11）, c = 15.027（3） , β = 121.22（3）°, V = 1606.6（6）？3, Dc = 2.468 g·cm-3, F（000） = 1168, μ = 7.122 mm-1, Z = 8, the final R = 0.0309 and wR = 0.0752 for 1763 observed reflections with I 〉 2σ（I）. For 2： monoclinic, space group P21/c with a = 8.7852（18）, b = 9.2744（19）, c = 9.752（2） , β = 103.45（3）°, V = 772.7（3）3, Dc = 2.410 g·cm-3, F（000） = 544, μ = 7.387 mm-1, Z = 4, the final R = 0.0321 and wR = 0.0741 for 1696 observed reflections with I 〉 2σ（I）. The structure of 1 shows a two-dimensional （4,4）-network composed of an inorganic ladder chain bridged by the phenyl-linkers of 4-apa ligands. Compound 2 exhibits a 3D layer-pillared framework with crb net, in which inorganic （4-82）-networks are joined by the phenyl-linkers.

关键词： synthesis crystal structure zinc arsonate

两种新型对氨基苯胂酸锌配位聚合物的合成和晶体结构

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两种新型对氨基苯胂酸锌配位聚合物的合成和晶体结构