Synthesis and Crystal Structure of [{Cd(hmbdc)(H_2O)_3}·2H_2O]_n

A novel coordination polymer [{Cd(hmbdc)(H2O)3}·2H2O]n (hmbdc = 5-hydroxy- isophthalic acid) has been synthesized and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c, with a = 9.599(3), b = 18.699(5), c = 7.557(2) , β = 108.198(4)°, V = 1288.6(6) 3, Z = 4, Mr = 382.60, Dc = 1.972 g/cm3, F(000) = 760, μ = 1.740, the final R = 0.0555 and wR = 0.0995 for 1732 observed reflections with I > 2σ(I). The structural analysis shows that the intermolecular hydrogen bonds and π-π interactions result in a three-dimensional supramolecular framework.     

Preconcentration of Ultra-trace Cadmium with Nanometer-size TiO2 Colloid and Determination by GFAAS with Slurry Sampling

Cadmium-a heavy metal used in coatings, batteries and plastics-can accumulate in human’s liver and kidney, causing osteoporosis and cancer1,2. The monitoring of its content is, therefore, of great importance. But the average concentration of cadmium in w…     

Synthesis and Crystal Structure of a Nitronyl Nitroxide Complex {[Zn(NIT4Py)(fum)(H2O)2]·H2}n

The title compound {[Zn(NIT4Py)(fum)(H2O)2]·H2O}n, where N1T4Py=2-(4'-pyridinyl)-4,4,5,5-tetra-methylimidazoline-l-oxyl-3-oxide and rum=fumarate, has been prepared and structurally characterized by X-ray diffraction. It crystallizes in triclinic, space group P1 with a =6.9533(9), b=9.805(1), c=15.248(2)A, a=94.608(2), β=92.328(2),γ=105.840(2)°,C16H24N3O9Zn, Mr=467.75, V=994.8(2) A3, Z=2, Dc=1.562 g/cm3,μ(MoKa)=1.289 mm-1,F(000)=486, the final R=0.0243 and wR=0.0622 for 3505 independent reflections with Rint=0.0125. The Zn(Ⅱ) adopts a distorted five-coordinate triangle bipyramidal geometry. The basic framework structure of the complex is a 1-D chain. The intrachain hydrogen bonds are helpful to stabilize the 1-D chain structure. Furthermore, the chains are connected by O-H…O hydrogen bonds to give a 2-D double-layer network.     

配合物[CdCl(HL)(dpp)(H2O)]n·nH2O的合成、晶体结构与荧光性能研究

Under hydrothermal condition, the reaction of 3-hydroxy-1-adamantaneacetic acid (H₂L) with CdCl₂ and 1,3-di-4-pyridylpropane (dpp) has afforded a new Cd(Ⅱ) compound, [CdCl(HL)(dpp)(H₂O)]_n·nH₂O(1), which was structurally characterized by single-crystal X-ray diffraction analysis. The crystal is triclinic, space group P1 with a=1.091 0(1) nm, b=1.131 8(1) nm, c=1.246 4(1) nm, α=88.52(1)°, β=71.34(1)°, γ=68.11(1)°, V=1.345 2(1) nm³, Z=2, M_r=591.40, F(000)=608, D_c=1.460 g·cm^-3, μ=0.947 mm^-1, the final R=0.040 1 and wR=0.104 0 for 4 950 observed reflections (I>2σ(I)). Complex 1 consists of one-dimensional chains deriving from CdCl(HL)(H₂O) units linked by dpp ligands, and lattice water molecules decorate between the chains. The O-H…O and O-H…Cl hydrogen bonds lead to the formation of a 2D layer structure. CCDC: 756099.     

Synthesis, Characterization and Crystal Structure of a Three-dimensional Coordination Polymer {[Cd(1,5-nds)(Him)2(H2O)]·2H2O}n

A novel cadmium(Ⅱ) coordination polymer {[Cd(1,5-nds)(Him)2(H2O)]·2H2O}n (1,5-nds = naphthalene-1,5-disulfonate and Him = imidazole) was synthesized based on the reaction of cadmium oxide and 1,5-naphthalenedisulfonic acid firstly, and then mixed with imidazole in methanol medium. Its structure was characterized by elemental analysis, IR and TGA, respectively. The crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P, with a = 8.5420(10), b = 10.2570(10), c = 13.361(2)(A), α = 100.704 (2), β = 100.195(2), γ = 108.873(3)°, C16H20Cd N4O9S2, Mr = 588.91, V = 1.0524(2) nm3, Dc = 1.858 g/cm3, Z = 2, F(000) = 592, μ= 1.294 mm-1, R = 0.0397 and wR = 0.1007 for 3180 observed reflections (I > 2σ(I)). Structural analysis shows that the cadmiun atom is coordinated with four oxygen atoms from three 1,5-nds and one water molecule together with two nitrogen atoms from two imidazoles, giving a distorted octahedral coordination geometry. The molecules are linked to form a two-dimensional coordination polymer based on bridging ligands of naphthalene-1,5-disulfonate anions, the sheets of which are then interacted via hydrogen bonds, leading to a three-dimensional network structure.     

Synthesis and Crystal Structure of [Zn(FcCOO)2(2,2′-bipy)(H2O)]2·H2O

A novel complex [Zn(FcCOO)2(2,2′-bipy)(H2O)]2·H2O (Fc = (η5-C5H5)Fe(η5-C5H4), 2,2′-bipy = 2,2′-bipyridine) has been synthesized and characterized by elemental analysis, IR and X-ray diffraction. It crystallizes in monoclinic system, space group P21/c with a = 6.8187(4), b = 21.7155(13), c = 19.7411(12) (A), α = 90, β = 97.7420(10), γ = 90°, C64H58Fe4Zn2N4O11, Mr = 1413.28, V = 2896.4(3) (A)3, Dc = 1.620 g/cm3, Z = 2, F(000) = 1444, μ(MoKα) = 1.857 mm-1, R = 0.0523 and wR = 0.0982 for 3219 observed reflections (I ＞ 2σ(I)). Structural analysis shows that the zinc atom is coordinated with three oxygen atoms from two ferrocenemonocarboxylates and one water molecule together with two nitrogen atoms from 2,2′-bipyridine, giving a distorted square-pyramidal coordination geometry. The complex molecules are linked to form an infinite one-dimensional chain by both intermolecular hydrogen bonds and π-π stacking interactions of the bipyridine rings.     

Synthesis and Crystal Structure of [Zn(FcCOO)_2(2,2'-bipy)(H_2O)]_2·H_2O

A novel complex [Zn(FcCOO)2(2,2'-bipy)(H2O)]2·H2O (Fc = (η5-C5H5)Fe(η5-C5H4), 2,2'-bipy = 2,2'-bipyridine) has been synthesized and characterized by elemental analysis, IR and X-ray diffraction. It crystallizes in monoclinic system, space group P21/c with a = 6.8187(4), b = 21.7155(13), c = 19.7411(12) A, α = 90, β = 97.7420(10), γ = 90o, C64H58Fe4Zn2N4O11, Mr = 1413.28, V = 2896.4(3) A3, Dc = 1.620 g/cm3, Z = 2, F(000) = 1444, μ(MoKα) = 1.857 mm-1, R = 0.0523 and wR = 0.0982 for 3219 observed reflections (I > 2σ(I)). Structural analysis shows that the zinc atom is coordinated with three oxygen atoms from two ferrocenemonocarboxylates and one water molecule together with two nitrogen atoms from 2,2'-bipyridine, giving a distorted square-pyramidal coordination geometry. The complex molecules are linked to form an infinite one-dimensional chain by both intermolecular hydrogen bonds and π-π stacking interactions of the bipyridine rings.     

多元混配合物[Ni(NPA)2(Phen)(Ac)(H2O)]·H2O的合成、晶体结构

0引言镍是生物体中必须的痕量元素,常成为一些酶的活性中心,因而模拟镍酶并研究其结构,一直是生物无机化学等领域的重要研究课题,近年来镍配     

Syntheses, Crystal Structures and Thermal Properties of Two Dicadmiun(Ⅱ) Complexes Cd2L2X2 (HL = N-(3-Methoxylsalicylidene)-3-dimethylaminopropylamine, X = CI (1), NCS (2))

Two Cd(Ⅱ) complexes, Cd2L2Cl2 (1) and Cd2L2(NCS)2 (2) (HL = N-(3-methoxyl- salicylidene)-3-dimethylaminopropylamine) were synthesized and determined by EA, IR, TG and single-crystal X-ray diffraction. The crystallographic data are as follows: monoclinie, space group P21/n, a = 9.2710(9), b = 18.0069(18), c = 18.5562(19) A, β= 99.741(4)°, V= 3053.1(5), Z= 4,μ = 1.605, F(000) = 1536, R = 0.0264 and wR = 0.0699 for 1; orthorhombic, space group Pca21 a = 16.196(3), b = 11.506(2), c = 36.126(7)A, V = 6732(2), Z = 8,μ = 1.428, F(000) = 3264, R = 0.0376 and wR = 0.0877 for 2. There are two geometrically different octahedral Cd(Ⅱ) atoms, with N4O2 and O4Cl2 donor sets for 1 while N4O2 and N2O2 for 2. In the dinuclear Cd(Ⅱ) centers, the Cd(Ⅱ) atoms are held together by two deprotonted phenolate oxygen atoms from tetradentate L ligands. The thermal gravity data show two step decompositions with the residues of CdO for two complexes.     

2D氢键网络镉配合物Cd(pyridine-2-sulfonato)2(H2O)2和锌配合物Zn(pyridine-2-sulfonato)2(H2O)2的合成和晶体结构

合成了镉的吡啶-2-磺酸配合物Cd(C5H4NSO3)2(H2O)2 1和锌的吡啶-2-磺酸配合物Zn(C5H4NSO3)2(H2O)2 2。 研究表明, 2个化合物属异质同晶, 均属单斜晶系, 空间群为C2/c. 化合物1晶胞参数为:a = 13.7671(5), b = 7.2778(3), c = 16.1559(9) ? b = 106.656(3)? V = 1550.8(1) 3, Z = 4, Dc = 1.990 g/cm3, m =1.719 mm-1, F(000) = 920, R = 0.0225, wR = 0.0584, 共收集到1759个独立衍射点, 其中I≥2(I)的可观测点为1681个;化合物2晶胞参数为:a = 13.711(1), b = 7.1451(9), c = 15.972(1) , b =107.079(5)? V = 1495.7(3) 3, Z = 4, Dc = 1.855 g/cm3, m = 1.964 mm-1, F(000) = 848, R = 0.0310, wR = 0.0831, 共收集到1707个独立衍射点, 其中I≥2(I)的可观测点为1592个。在2个标题配合物中, Cd2+离子(或Zn2+离子)由2个吡啶-2-磺酸中的2个氮和2个氧以及2个水分子中的2个氧配位形成畸变的N2O4八面体配位构型。每个配合物分子具有晶体学2次旋转轴对称性。配合物分子之间通过许多OH(配位水分子)LO(未配位磺酸根)氢键联结成二维结构网络。     

超分子化合物[Cu(Phen)(C2O4)H2O]·H2O的合成及结构

邻菲罗啉配合物具有良好的光化学、电化学、催化性质和生物活性[1-4],因而引起了人们的极大关注[5-7]。我们利用Phen和K2[Cu(C2O4)2],通过取代反应合成了标题配合物,并对其进行了结构分析,结果表明,中心铜原子处在五配位的变形四方锥环境中,且晶体中结构单元通过分子间氢键形成     

Synthesis of A New Reagent 1-(6-Nitro-2-Benzothiazolyl)-3-(4-Nitrophenyl)-Triazene and Study on Its Color Reaction with Cadmium

Thetriazenereagentswereusedf0rthedeterminationofcadmium,mercuryandzinc.Somereagentscontainingdiaz0amin0az0benzenehavebeenreported'-'.Wehavesynthesizedreagentscontainingdiaz0aminonitrobenzene4'5.Recently,anewreagentNBTNPThasbeensynthesizedin0urlab0ratoryanditscolorreactionwithcadmiumwasstudied.Resultsshowthatthisreagenthashighsensitivitywithmetallicions.Theproposedmeth0dhasbeenaPpliedt0thedeterminati0nofcadmiuminhumanhairandwastewaterwithsatisfact0ryresults.Theprocedureofsynthesis0fNBTNPT…     

混合配体的铜(Ⅱ)配合［Cu(C2H4O2N)(C12H8N2)(H2O)］.ClO4.2.5H2O的合成、性质及晶体结构

本文对甘氨酸、1,10 -邻菲咯啉铜 ( )固体配合物进行了合成和表征 ,并利用 X射线分析研究了其晶体结构     

一维链状配位聚合物[Zn(bipy)(H2O)2SO4]的合成及晶体结构表征

配位聚合物有迷人的拓扑学结构和不同寻常的物理、化学性质,它们在主客体化学、磁性材料、超导材料、非线性光学材料、催化及生物活性等诸多方面都表现出极好的应用前景,吸引了许多国内外学者投入到这一领域进行研究[1-4]。到目前为止,人们已经制备出了大量的配位聚合物,并对其     

二聚体[Ni(TSSB)(Phen)(H_2O)]·4H_2O的合成、表征、晶体结构及热分解研究

0引言含硫席夫碱及其金属配合物具有抑菌、抗癌和抗病毒的生物活性[1￣3],有些含O、N席夫碱金属配合物具有仿酶催化活性[4,5]。而氨基酸席夫碱配合物具有良好的生物生理活性,近年来得到人们的普遍重视[6,7],同α-氨基酸席夫碱相比,β-氨基酸席夫碱由于氨基位置的变化而引起不同     

Syntheses and Structures of Two New Cobalt Supramolecular Complexes, [Co(4,4'-bipy)_2(H_2O)_4]· [Co_2(4,4'-bipy)3O(H_2O)_8]·2TST·2(4,4'-bipy)·4H_2 and [Co(4,4'-bipy)_2(H_2O)_4]DSNT'4,4'-bipy

Two new cobalt(Ⅱ) supramolecular complexes [Co(4,4'-bipy)_2(H_2O) _4]·[Co_2(4,4'-bipy)3-(H_2O) _8]·2TST-2(4,4'-bipy)·4H_2O 1 and [Co(4,4'-bipy) _2(H_2O) _4]DSNT·4,4'-bipy 2 based upon the assembly of Co(Ⅱ), 4,4'-bipyridine (4,4'-bipy) and two new multifunctional organic ligands, 2,4,6-tris(4-sulfophenyl-amino)-1,3,5-triazine (H_3TST) and 2,4-bis(p-sulfanilato)-6-diethylamino-1,3,5-triazine (H_2DSNT), have been prepared by hydrothermal method and characterized by elemental analysis, IR spectrum, and single-crystal X-ray diffraction. The crystal structure of 1 is of monoclinic, space group P2_(1/n) with α= 13.599(4), b = 18.988(6), c = 22.995(7) A, β = 90.273(6)°, V= 5938(3) A~3, Z = 4, C_(56)H_(59)CO_(1.5)N_(13)O_(17)S_3, M_r = 1370.74, D_c = 1.533 g/cm~3,μ = 0.613 mm~(-1), F(000) = 2842, GOOF = 1.018, the final R = 0.0796 and wR = 0.1498 for 9019 observed reflections with I > 2o(I). The crystal structure of 2 belongs to the monoclinic system, space group C2/c with α = 18.864(6), b = 14.283(5), c = 20.246(7) A, β = 107.799(6)°, V = 5194(3) A~3, Z = 4, C_(49)H_(52)CoN_(12)O_(10)S_2, M_r = 1092.08, D_c = 1.397 g/cm~3, μ= 0.480 mm~(-1), F(000) = 2276, GOOF = 1.059, the final R = 0.0665 and wR = 0.1900 for 4887 observed reflections with I> 2σ(I). The results of X-ray crystal structure analysis revealed that complexes 1 and 2 exhibit layered supramolecular frameworks stabilized by electrostatic interactions, π-π interactions and hydrogen bonds.     

Solvothermal Synthesis, Crystal Structure and Electrochemical Property of Complex [Co(p-MBA)2(2,2'-bipy)(H2O)]·(H2O)

One novel complex [Co(p-MBA)2(2,2'-bipy)(H2O)]·(H2O) has been synthesized by the reaction of p-methylbenzoic acid with 2,2'-bipyridine in the solvent mixture of water and methanol. It crystallizes in triclinic, space group P-1 with a=0.70479(14), b=1.1211(2), c=1.6718(3) nm, α=103.806(3), β=90.795(3), γ=104.207(3)°, V=1.2399(4) nm3, Mr=512.41, Dc=1.373 g/cm3, Z=2, F(000)=532, μ=0.733 mm-1, R=0.0432 and wR=0.0957. The crystal structural analysis shows that the cobalt atom is coordinated with three oxygen atoms from two p-methylbenzoic acids and one water molecule and two nitrogen atoms from one 2,2'-bipyridine,forming a distorted square-pyramidal coordination geometry. The cyclic voltammetry behavior of the complex is also reported.     

{Cd(dmt)_2(Hchdc)_2(H_2O)_2}_n配合物的合成与表征

通过水热合成的方法,以1,4-环己烷二羧酸、2,4-二氨基-6-甲基三嗪和CdCl_2·2.5H_2O为原料合成了一种单核的化合物{Cd(dmt)_2(Hchdc)_2(H_2O)_2}_n(dmt=2,4-diamino-6-methyl-triazine,H2chdc=1,4-cyclohexanedicarboxylic acid),并进行了IR和X射线单晶衍射(常温)的分析.结果表明,该化合物属于P2/c空间群,单斜晶系,晶胞参数:a=1.330 26(11)nm,b=0.541 47(4)nm,c=2.415 54(16)nm,β=115.751(3)°,V=1.567 1(2)nm~3,Z=2,Dc=1.570g/cm~3,F(000)=764,R1=0.035 2,wR2=0.092 7.该化合物中,中心金属离子Cd(II)与氧相连形成六配位构型,并通过4种不同的氢键作用最终形成了三维的堆积结构.     

Solvothermal Synthesis,Crystal Structure and Electrochemical Property of Complex [Co(p-MBA)_2(2,2′-bipy)(H_2O)]·(H_2O)

One novel complex [Co(p-MBA)2(2,2′-bipy)(H2O)]·(H2O) has been synthesized by the reaction of p-methylbenzoic acid with 2,2′-bipyridine in the solvent mixture of water and methanol. It crystallizes in triclinic,space group P1 with a=0.70479(14),b=1.1211(2),c=1.6718(3) nm,α=103.806(3),β=90.795(3),γ=104.207(3)o,V=1.2399(4) nm3,Mr=512.41,Dc=1.373 g/cm3,Z=2,F(000)=532,μ=0.733 mm-1,R= 0.0432 and wR=0.0957. The crystal structural analysis shows that the cobalt atom is coordinated with three oxygen atoms from two p-methylbenzoic acids and one water molecule and two nitrogen atoms from one 2,2′-bipyridine,forming a distorted square-pyramidal coordination geometry. The cyclic voltammetry behavior of the complex is also reported.     

一维链状配合物Cd(SDBA)(H_2O)_2的合成及其晶体结构

用水热法合成了新型的一维配合物Cd(SDBA)(H2O)2(1,H2SDBA=二苯砜-4,4'-二甲酸),其结构经IR,元素分析和X-射线单晶衍射表征.1属于单斜晶系,P2/c空间群,晶胞参数: a=1.330 3(6) nm,b=0.528 2(9) nm,c=1.217 6(6) nm,β=116.143(5)°,V=0.768(6) nm3,Z=2,Mr=452.7 g·mol-1,Dc=1.958 g·cm-3,μ=1.599 mm-1,F(000)=448,R1=0.041 3,wR2=0.098 3,S=0.985. 1中Cd2+与2个SDBA2-配体上的4个O原子和2个配位水上的2个O原子配位,形成一个畸变的八面体.在a轴方向,Cd2+经SDBA2-桥联形成一维波浪状链,链与链之间通过氢键相互作用形成三维超分子结构.