A New Cadmium(Ш) Polymer Based on 3,5-Pyrazoledicarboxylic Acid:Hydrothermal Synthesis and Crystal Structure

The reaction of CdCl3.2.5H2O with 3,5-pyrazoledicaiboxylic acid under hydrother-mal conditions produce a novel three-dimensional（3-D） coordination polymer [Cd2（C5H2O4N2）2.2H2O]n.The title compound crystallizes in the monoclinic system,space group P21/c with a = 6.422（4）,b = 12.334（7）,c = 8.936（6） ,β = 104.793（7）°,V = 684.4（7） 3,Z = 4,Dc = 2.761 g/cm3,μ = 3.181 mm-1,F（000） = 544,R = 0.0248 and wR = 0.0624.In the crystal structure of the title compround,molecules are linked through N-H...O hydrogen bonds,forming chains running along the a axis.Every Cd（Ш） coordinates with four molecules of ligand and one water molecule,forming a pentagomal-bipyramidal geometry.

Hydrothermal Synthesis, Crystal Structure and Photoluminescence of [Sm(PCA)_3(H_2O)_2]_n·6nH_2O

A new one-dimensional （1-D） compound [Sm（PCA）3（H2O）2]n·6nH2O （1, HPCA=pyrazinecarboxylic acid） has been synthesized via hydrothermal reaction and structurally characterized by single-crystal X-ray diffraction. Compound 1 crystallizes in the Pbca space group of orthorhombic system with a=19.465（3）, b=12.034（4）, c=19.842（4） , V=4648（2）3, C15H25N6O14Sm, Mr=663.76, Dc=1.897 g/cm3, S=1.023, μ（MoKα）=2.610 mm-1, F（000）=2648, R=0.0239 and wR=0.0616. Compound 1 is characteristic of an infinite 1-D chain-like structure with the samarium atoms locating at an environment of a monocapped square antiprism. The [Sm（PCA）3（H2O）2]n chains and the lattice water molecules interconnect together through π-π interactions and hydrogen bonding interactions to yield a 3-D supramolecular framework. Photoluminescent investigation reveals that the title compound displays an emission in the greenish blue region.

Hydrothermal Synthesis, Crystal Structure and Fluorescence Property of a Novel Coordination Polymer [Eu_2(C_6H_8O_4)_3(H_2O)_2]_n·n(4,4′-bpy)

A novel coordination polymer [Eu2(C6H8O4)3(H2O)2]n?n(4,4?-bpy) (Mr = 928.51) was synthesized by the hydrothermal reaction of EuCl3?6H2O, adipic acid and 4,4?-bpy, and determined by elemental analysis, IR spectroscopy, thermal gravimetric analysis, single-crystal diffraction and fluorescence property. X-ray analysis reveals that a three-dimensional network has been formed between Eu3+ by carboxyl of adipic acid. The crystal is of orthorhombic, space group Pbcn with a = 21.870(7), b = 7.652(2), c = 19.624(6) ?, V = 3284.1(17) ?3, Z = 4, Dc = 1.878 g/cm3, μ = 3.854 mm-1, F(000) = 1824, R = 0.0345 and wR = 0.0565. The coordination polymer exhibits intensive red light under UV excitation at room temperature, which is attributed to the 5D0→7F2 transition of Eu(Ⅲ) ions.

Synthesis, Crystal Structure and Property of Cu Pb_2(OH)_2Cl_3

A new copper（1）-lead（Ⅱ） oxyhalide, CuPb2（OH）2Cl3, has been prepared by hydrothermal reaction and structurally characterized by single-crystal X-ray analysis. The compound crystallizes in tetragonal, space group 14（1）/acd with a = b = 13.77（1）, c = 15.38（1） A, V = 2916.2（2）, Z = 4, Mr = 618.29, Dc = 5.633 g/cm^3,μ = 49.97（2） mm^-1, F（000） = 4192, the final R = 0.0204 and wR = 0.0452 for 757 observed reflections with I 〉 2σ（I）. The structure of CuPb2（OH）2Cl3 contains one-dimensional helical chains built by CuCl4 tetrahedra with comer-sharing along the c-axis, in which the Pb^2＋ and OH^- ions are located at the voids between chains. Optical reflectance spectrum measurements indicate that it is a semiconductor with a band-gap of 3.23 eV.

Two New Coordination Polymers Assembled with a Functionalized Ligand:Syntheses and Crystal Structures

Two new transition-metal organic coordination polymers [M（mna）2]（M = Cd（1）,Zn（2）;mna = 2-mercaptonicotinic anion） have been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction along with IR and elemental analyses.Compound 1 is generally a one-dimensional linear structure bridged through the sulfur donor of mna ligand,while 2 is a one-dimensional zigzag chain ligated via the oxygen donor of mna ligand.These compounds further result in three-dimensional structures via intermolecular π...π stacking interactions and/or hydrogen bonding interactions.The two compounds were structurally determined by single-crystal X-ray diffraction.Complex 1 crystallizes in monoclinic space group P21/c with a = 3.730（3）,b = 13.973（12）,c = 12.380（11） ,β = 97.953（18）°,V = 639.0（10） 3,Z = 2,CdC12H8O4N2S2,Mr = 420.72,Dc = 2.187 g/cm3,F（000） = 412,Rint = 0.0252,T = 293（2） K,μ = 2.052 mm？1,the final R = 0.0269 and wR = 0.0586 for 1377 observed reflections with I 2σ（I）.Complex 2 belongs to monoclinic space group P21/c with a = 13.376（2）,b = 12.8429（14）,c = 7.4856（10） ,β = 96.190（10）°,V = 1278.5（3） 3,Z = 4,ZnC12H8O4N2S2,Mr = 373.69,Dc = 1.941 g/cm3,F（000） = 752,Rint = 0.0414,T = 293（2） K,μ = 2.264 mm？1,the final R = 0.0418 and wR = 0.0966 for 2396 observed reflections with I 2σ（I）.

MnQ_2(Q=S,Se,Te)and Te_4 Structures and Their Semiconductor Properties

The solvo―thermal technique is used for the synthesis of [Mn(en)_3]Te_4 (I).The crystal structure has been determined by single crystal X―ray diffraction techniques. Thecrystal belongs to the monoclinic, space group p2_1/c with unit cell:a = 0. 846 1(1), b=1.5653(2),c=1.426 9(2) nm, α = 90°, β=91. 37(1) (3)°, γ=90°, V=1. 889 3(4) nm^3, and Z=4. The resultsshow that the structure contains a linear chain Zintl anion, [Te_4 ]^(2-) and a complex cation,[Mn(en)_3l^(2+). Optical studies have been performed on the powder sample of I, suggesting that thecompound is a semiconductor with a band gap of 0. 73 eV. The semiconductor properties for MnQ_2(Q=S, Se, Te) and [Mn(en)_3]Te_4 have been discussed by molecular orbital theory.

Reaction in situ found in the synthesis of a series of lanthanide sulfate complexes and investigation on their structure, spectra and catalytic activity

A series of lanthanide sulfates coordination complexes, Ln2(SO4)3(H2O)8 (Ln = Pr (1), Nd (2), Tb (3), Sm (4), Dy (5), Gd (7), Ho (8)), and EuK(SO4)2 (6), were constructed by the reaction in situ of lanthanide ions (Ln3+) with flexible dodecanedioic acid and rigid aromatic 5-sulfosalicylic acid under hydrothermal conditions. All of them were characterized by elemental analysis, IR spectroscopy, and single-crystal X-ray diffraction. The crystal structures and coordination modes of metal centers and sulfate ions, as well as the novel reaction mechanism and different conditions of lanthanide ions and 5-sulfosalicylic acid to form the series of lanthanide sulfate complexes, were discussed in detail. Solid-state properties for these crystalline materials, such as thermal stability and powder X-ray diffraction have been investigated. Additionally, the photoluminescent characterizations of the complexes 3, 4, 5 and 6, and the catalytic properties of all the complexes about cyclohexane being oxidized into cyclohexanone/cyclohexanol were investigated and compared.

Synthesis,Structure,and Magnetic Properties of a New Cobalt Selenite Ca_2Co(HSeO_3)_2(SeO_3)_2

A new cobalt selenite,Ca_2Co（HSeO3）_2（SeO_3）_2,was synthesized by a conventional hydrothermal method. Single-crystal X-ray diffraction analysis reveals that Ca_2Co（HSeO3）_2（SeO_3）_2 crystallizes in triclinic system,space group P1,with a = 5.330（5）,b = 7.047（7）,c = 8.457（9） ？,V = 285.0（5） ？~3,Z = 1,Mr = 646.93,Dc = 3.769,μ = 15.235 mm^（-1）,F（000） = 299.0,the final R = 0.0452 and wR = 0.1169 for observed 1265 reflections with I 〉 2σ（I）. The title compound consists of isolated chains built from CoO_6 octahedra and SeO_3 pyramids. In this structure,the chains are separated by Ca^（2＋） cations. Magnetic measurements confirm that the title compound exhibits long-range antiferromagnetic ordering at 3 K and field-induced magnetic transition at 2 T.

Syntheses, Structures, and Some Properties of Three Vanadium Selenites

Three novel vanadium selenites with the formulae [（VO2）（1,10-phenanthtoline）（SeO3H）]2 1, [（VO2）（2,2′-bipyridine）]2（SeO3） 2 and [（VO）（H2O）（SeO3）2]2（HaEDD） 3 （EDD = N1,N1′-（ethane-1,2-diyl）diethane-1,2-diamine） were hydrothermally synthesized, and characterized with elemental analysis, FT-IR spectrum, Raman spectrum, TG-DTA analysis, EPR spectra, and single-crystal X-ray diffraction analysis. Compound I belongs to the triclinic system, space group P1^- with a = 7.7527（5）, b = 9.5345（10）, c = 9.8192（8） A^°, α = 92.712（3）, β = 105.540（3）, γ = 108.154（4）°, V = 657.66（1） A^°^3, Mr = 782.22, Z = 1, F（000） = 384,μ（MoKa） = 3.544 mm^-1, R = 0.0432 and wR = 0.1142; Compound 2 is of orthorhombic system, space group F212121 with a = 7.6574（15）, b = 14.916（3）, c = 19.085（4） A, V = 2179.8（8） Aa, Mr = 605.21, Z = 4, F（000） = 1200, μ（MoKa） = 2.579 mm^-1, R = 0.0338 and wR = 0.0658; Compound 3 belongs to the triclinic system, space group P1^- with a = 9.247（2）, b = 9.659（2）, c = 7.2651（19） A^°, α = 98.171（7）, β = 103.709（5）, γ = 114.712（13）°, V = 550.9（2） A^°^3, Mr = 828.03, Z = 1, F（000） = 400, μ（MoKa） = 7.537 mm^-1, R = 0.0641 and wR = 0.2118. Compound 1 is constructed from alternating corner-shared [VO4N2] octahedra and SeO3H units, forming a dimeric vanadium unit. These assemblies are further linked into an infinite chain via hydrogen bonds along the a axis. In the structure of 2, two distinct V centers form centrosymmetric [V2O6N4] clusters through edge-sharing, and the SeO3 unit serves as a capping unit to fix the oxovanadate cluster. In the structure of 3, each [VO6] octahedron shares four oxygen atoms with adjacent Se atoms, while every SeO3 unit shares two oxygen atoms with neighboring V atoms. This connectivity of alternating VO6 and SeO3 units results in a joint-like chain. Based on the TGA analysis, these three compounds are thermally stable under 200℃ .

Synthesis, Structure, and Magnetic Properties of a New 2D Cobalt(Ⅱ) Metal-organic Framework

Rational design of magnetic materials with desired magnetic properties has attracted wide interest in recent decades. Herein, we present a new 2D cobalt（II） metal-organic framework, namely [Co（MQ）2（V2O6）2]n·4nH2O 1, which was hydrothermally synthesized by the reaction of Co（NO3）2·4H2O, N-methyl-4,4′-bipyridinium（MQ＋） chlorine salt and NH4VO3. Single-crystal X-ray diffraction analysis reveals that 1 crystallizes in C2/c space group with a = 16.290（5）, b = 7.815（2）, c = 25.297（7） A, β = 108.459（5）°, V = 3054.8（15） A3, Z = 4, Dc = 1.890 g/cm3, μ = 1.791 mm-1, F（000） = 1748, the final R = 0.0444 and wR = 0.1208 with I 〉 2σ（I）. The individual Co（II） is connected and well separated by diamagnetic [V2O6]2-linkers. Magnetic measurements confirm that 1 exhibits ferrimagnetic interactions.

A Metal-organic Framework Containing Octanuclear Zn(Ⅱ) Clusters Constructed by 5-Methoxyisophthalate and Flexible Bis(imidazolyl) Ligand

The hydrothermal reaction of 5-methoxyisophthalic acid（MeO-H2ip）, 1,3-bis（2-methylimidazol-1-yl）propane（bmip） and Zn（NO3）2·6H2O in the presence of NaOCH3 gave rise to a three-dimensional（3-D） metal-organic framework containing octanuclear Zn（II） units, [Zn4（MeO-ip）3（OH）2（bmip）]n. Single-crystal X-ray diffraction analysis reveals that the complex crystallizes in the triclinic space group P1 with a = 11.348（3）, b = 14.163（4）, c = 15.088（4） , α = 108.537（2）, β = 106.542（2）, γ = 103.106（1）o, V = 2065.4（9） -3, Z = 2, Mr = 334.62, Dc = 1.740 g·cm-（-3）, μ = 2.375 mm-（-1）, S = 1.015, F（000） = 1096, the final R = 0.0272 and w R = 0.0715 for 8929 observed reflections（I 〉 2σ（I））. The complex is thermally stable up to 370 oC, and exhibits photoluminescent emission at 450 nm on 350 nm excitation.

新型三维配位聚合物[Fe(C_5H_4NCOO)_2]_n的可控合成、晶体结构和UV-VIS-NIR反射光谱研究

A novel coordination polymer, [Fe(C 5H 4NCOO) 2] n, was synthesized by hydrothermal reaction and characterized by elemental analysis as well as IR spectroscopy. The crystal structure (with a novel 3-D network) of this compound belongs to monoclinic, space group P2 1/n, a=0.49544(1) nm, b=1.32443(2) nm, c=1.04983(1) nm, β=101.586(1)°. The diffuse reflectance spectra (200～2500 nm) showed that the polymer had strong absorbance in 375～563 nm (E g≈2.5 eV) region and weak absorbance from 720 to 2500 nm (near infrared spectra).

三维配位聚合物[Co(pda)(SCN)(H_2O)]_n[pda=3-(3-吡啶基)丙烯酸]的合成和晶体结构

以CoCL_2、3-(3-吡啶基)丙烯酸(pda)和KSCN为原料,在水热反应条件下,合成了一种三维配位聚合物[Co(pda)(SCN)(H_2O)_n]晶体,对其进行了元素分析、红外光谱表征、X射线单晶衍射测定和热重分析。该配位聚合物属三斜晶系,P-1空间群,晶胞参数为a=0.7309(5)nm,b=0.8799(6)nm,c=0.9634(6)nm,α=68.128(10)°,β=73.241(11)°,γ=71.218(12)°,V=0.5343(6)nm^3,Z=2,d_c=1.760g/cm^3,μ=1.792mm^(-1),F(000)=268,R1=0.0450,wR2=0.1035。X射线单晶衍射显示形成一个三维的网络结构。

具有生物活性的1,4-二氢吡啶衍生物的水热法合成及结构表征

A series of 1,4-dihydropyridine derivatives were synthesized by the reaction of aromatic aldehydes,ethyl acetoacetate and ammonium bicarbonate under hydrothermal condition.Compared to the known report,this method has the advantages of excellent yields,convenience,less pollution and friendly environment.Compound b was deterimined by X-ray single-crystal diffraction.The crystal is of monoclinic,space group C2/c with a = 19.7348(12),b=7.4285(4),c = 27.2561(16),β=106.9950(10)°,V=0.38212(4)nm3,Z=8,Dc =1.236 Mg/m3,μ=0.085 mm-1,F(000)=1520,S=1.053,R=0.0574,wR=0.1732.

一个中心对称的(6,3)拓扑二维蜂窝网的Ni-咪唑基三脚架配合物的合成、结构及其介电性

利用水热合成法,以金属盐NiSO4·6H2O与三脚架配体1,3,5-三(1-咪唑基)苯(tib)进行组装,得到了一个结构新颖的有序金属-有机框架(MOFs){[Ni3(tib)2(H2O)12](SO4)3}n(1).利用X-射线单晶衍射仪检测其晶体结构,并进行元素分析,红外光谱射线,粉末衍射等相关表征.配合物1为一个典型的(6,3)拓扑二维蜂窝网结构,由于π-π空间叠加效应和氢键相互作用形成了稳定的三维结构.对配合物1介电性能进行测定,发现其在138℃时达到最大的介电异常值10.08,为典型的介电材料,通过热重分析,表明此材料具有较好的热力学稳定性,对新型多维MOFs及新型介电性能材料的开发具有借鉴和指导意义.

多纳米孔道配位聚合物[Cd(pda)_2]_n的合成与晶体结构

以Cd(CH3COO)2.2H2O和3-(3-吡啶基)丙烯酸(pda)为原料,在水热合成反应条件下,合成了一种新型多纳米孔道的二维配位聚合物[Cd(pda)2]n。对其进行了元素分析、红外光谱表征、差热-热重分析和X射线衍射测定。结果表明:该配位聚合物属三斜晶系,P-1空间群,它为一个二维结构,在220℃下呈稳定结构。

4′-(4-苯甲酸)-2,2′：6′,2″-三联吡啶锌配位聚合物的合成、晶体结构及荧光性质研究

本文用水热法合成一个新型的锌配合物{[Zn2(ttp-COO)(MoO4)(OH)]·2H2O}n(ttp为4′-(4-苯甲酸)-2,2′:6′,2″-三联吡啶)。X-射线单晶衍射分析表明,该配合物晶体属三斜晶系,空间群为P-1,晶胞参数为:a=0.799 92(4)nm,b=1.215 35(6)nm,c=1.279 28(6)nm,α=82.234 0(10)°,β=72.168 0(10)°,γ=80.657 0(10)°,V=1.163 40(10)nm^3,Z=2,最后一致性因子R1=0.033 5,wR2=0.094 2。在配合物中,有2个晶体学上独立的锌原子,其中Zn1(Ⅱ)与配体提供的3个氮原子、钼酸根离子的1个氧原子及水分子结合,形成五配位的四角锥形,Zn2(Ⅱ)与配体中羧酸根离子的1个氧原子、钼酸根离子的2个氧原子,以及μ2-OH基团结合,成四面体构型。本文还对该配合物进行了荧光和热重表征。

具有二重穿插结构的配位聚合物[Cu(bpy)(OH)]_n的合成与结构表征

利用水热反应,合成了一个具有二重穿插结构的一价铜配位聚合物[Cu(bpy)(OH)]n(1)(bpy=4,4'-联吡啶),并利用元素分析,X射线单晶衍射,红外光谱以及热重分析等手段对标题化合物进行了表征.晶体学数据:四方晶系,I41/acd空间群,a=1.41802(6)nm,b=1.41802(6)nm,c=3.8568(3)nm,β=90.00°,V=7.7552(7)nm3,Z=32,S=1.074,最终残差因子[I>2σ(I)]R1=0.0345,wR2=0.0767,对于全部数据R1=0.0566,wR2=0.0867.

3,4-苯并咪唑酰肼的水热合成及其结构和荧光性能表征

采用水热合成法,经由反应物之间的酰胺化反应,合成出3,4-苯并咪唑酰肼C9H7N4O2(1).通过单晶X-射线衍射法对其结构进行表征.结构解析表明,化合物1属于单斜晶系,P21/n空间群,晶胞参数a=0.367 47(3)nm,b=1.407 84(6)nm,c=1.528 50(7)nm,α=90°,β=95.095(7)°,γ=90°,V=0.787 63(7)nm3,Z=4,R1=0.054 7,ωR2=0.113 3.并对化合物1进行了元素分析、红外光谱分析和荧光性质的测试.

具有强绿色荧光发射效应的2,2′-二硝基4,4′-联苯酸铀(Ⅵ)配聚物(英文)

A very complex 3D Uranium(Ⅳ) metal-organic framework was obtained by the hydrothermal treatment of UO2(NO3)2·6H2O with (R,S)-2,2′-dinitro-biphenyl-4,4′-dicarboxylic acid (BTNCA) (L) in water at 180 ℃ in Pyrex tubes. The crystal belongs to monoclinic system with space group P21/c, and a=0.545 90(3) nm, b=3.676 01(18) nm, c=2.659 81(13) nm, β=91.4060(10)°, V=5.335 9(5) nm3, Z=4. CCDC:659615.