Helical Coordination Polymer with a 3-Fold Interpenetration Structure Based on 5-(Hydroxymethyl)isophthalic Acid

5-（Hydroxymethyl） isophthalic acid （H2HIA） as a novel organic ligand was prepared from 3,5-bis（methoxycarbonyl）benzoic acid by a two-step method. And then, a 3D helical coor- dination polymer with a 3-fold interpenetration structure, namely [Zn1/2（HIA）1/2（DPEE）1/2]n （1）, was hydrothermally synthesized at 160 ℃, using H2HIA ligands to assemble with DPEE ligands and Zn2＋ ions. Complex 1 crystalizes in orthorhombic system, space group Pnna, with a = 8.2118（5）, b = 17.1698（7）, c =14.9922（7） ？, V = 2113.82（18） ？3, μ = 1.194 mm-1, Z = 4 and S = 0.967. Moreover, some physical characteristics of complex 1, such as powder X-ray diffraction （PXRD）, thermogravimetry analyses （TGA） and photoluminescent properties, were also investigated.

Synthesis, Crystal Structure and Properties of a Chiral 3D Supramolecular Coordination Polymer [Co(HL)·(DMF)]_n from 5-(Imidazol-1-ylmethyl)isophthalic Acid

A chiral supramolecular coordination polymer, [Co（HL）·（DMF）]n（1）, with helical chains from a flexible ligand 5-（imidazol-1-ylmethyl）isophthalic acid（H2L） has been obtained under hydrothermal conditions and characterized by elemental analysis, powder X-ray diffraction（PXRD）, IR, Uv/vis spectra, thermal gravimetric analyses（TGA） and also by single-crystal X-ray diffraction. It crystallizes in hexagonal, space group P6522 with a = 8.8109（3）, b = 8.8109（3）, c = 71.771（3） , γ = 120°, V = 4825.3（3） -3, Z = 6, Mr = 695.55, Dc = 1.436 g/cm-3, Rint = 0.0684, F（000） = 2166, the final R = 0.0923 and w R = 0.2697 for 3056 observed reflections（I 2σ（I））. The title coordination polymer 1 shows a chiral layered structure based on right-handed helix chains. Such layers are associated together through hydrogen-bonding interactions to form a 3D supramolecular framework.

Syntheses, Crystal Structures and Properties of Two Metal-organic Complexes Based on 5-(4-Pyridyl)-methoxyl Isophthalic Acid

Two new metal-organic frameworks, [Co3L2（NO2）2（H2O）2],, （1） and{[Ni（L）（H2O）5] （H2O）2.DMF}, （2, H2L = 5-（4-pyridyl）-methoxyl isophthalic acid）, have been synthesized by the hydrothermal method and characterized by elemental analysis, infrared spectroscopy, thermogravimetric analysis （TGA） and X-ray crystallography. Compound 1 crystallizes in the monoclinic system with space group P2/c and adopts a slightly distorted octahedral configuration. In compound 1, the 2D bilayered structures are linked by O-H...O and O-H...N hydrogen bonds to form a 3D framework. Compound 2 crystallizes in the monoclinic system with space group P2/n, and the central nickel atoms are octa-coordinated with five O atoms from coordinated water molecules and one N atom from one H2L ligand. The abundant O-H…O hydrogen bonds and π…π interactions link the molecules into a 3D framework. In addition, compounds 1 and 2 exhibit strong ultraviolet absorption in the solid state at room temperature.

Syntheses and Crystal Structures of One-dimensional Ni(Ⅱ) Complexes with 5-Tert-butyl Isophthalic Acid

Two new Ni（ Ⅱ） coordination polymers, {[Ni（tbip）（bipy）（H2O）]-0.5H2O}n 1 and [Ni（tbip）（phen）（H2O）]n 2 （Hatbip = 5-tert-butyl isophthalic acid, bipy = 2,2＇-bipyridine, phen = 1,10-phenanthroline）, have been synthesized under hydrothermal conditions and characterized by elemental analysis, X-ray diffraction, and IR spectroscopy. In the two polymers, H2tbip acts as a tridentate ligand. Compound 1 has a tbip bridged 1-D linear chain which is extended by hydrogen bonds into a 1-D double chain, while compound 2 exhibits a 1-D zigzag chain.

Syntheses and Characterizations of Cd(Ⅱ) and Pr(Ⅲ) Complexes Based on 5-(Tetrazol-5-yl) Isophthalic Acid

Hydrothermal reactions of 5-（tetrazol-5-yl） isophthalic acid with cadmium nitrate/praseodymium nitrate led to two complexes of [Cd3（TZI）2（H2O）（11）]n（1） and [Pr（TZI）（H2O）5]n（2）. Their structures and properties were determined by X-ray diffraction, IR spectroscopy, fluorescence spectrum, thermal gravimetric analyses and elemental analysis. Complex 1 belongs to monoclinic system, I2/c space group, with a = 12.8688（3）, b = 18.0925（3）, c = 14.5190（3）A, β = 116.054（3）°, V =3036.92（13） A^3, Z = 4; complex 2 crystallizes in triclinic, space group P 1, with a = 7.9690（5）, b =9.7665（8）, c = 10.4353（9） A, α = 116.709（9）, β = 107.461（6）, γ = 95.671（6）°, V = 665.54（9）A^3 and Z =2. Complex 1 is a 3D planar structure. Complex 2 is a one-dimensional double chain configuration and extends into a 3D network by hydrogen bonds and π-π interactions.

A Zn(Ⅱ) Coordination Polymer Based on a Flexible Polycarboxylate Ligand 5-(4-Hydroxypyridinium-1-ylmethyl)-isophthalic Acid: Synthesis, Structure, and Property

A Zn（Ⅱ） supramolecular coordination polymer, {[Zn2（L）2（m-bix）（H20）]6H2O}n（1）, with an interesting 1D→2D polythreading array from a flexible and angular organic aromaticpolycarboxylate ligand 5-（4-hydroxypyridinium-l-ylmethyl）isophthalic acid （H2L）, and N-donorligand 1,3-bis（imidazol-l-ylmethyl）benzene （m-bix）, has been obtained under hydrothermalconditions and characterized by elemental analysis, powder X-ray diffraction （PXRD）, IR, thermalgravimetric analyses （TGA） and single-crystal X-ray diffraction. In 1, the Zn（Ⅱ） center has twocoordination geometries. One exhibits a trigonal bipyramidal coordination sphere, and the other isa tetrahedral geometry; L2- has two different coordination modes, with one connecting three Zn（Ⅱ）ions through two monodentate carboxylate groups and the monodentate hydroxyl group, and theother bridging two Zn（Ⅱ） ions through two carboxylate groups. The L2- anions connect the Zn（Ⅱ）centers forming an infinite 1D tubular structure. These 1D tubes are interconnected by the m-bixspacers to form a 2D framework. Such 2D layers are further assembled into a 3D supramolecularnetwork via hydrogen bonds. Meanwhile, the luminescent property of 1 has also been investigatedin detail.

Synthesis,Crystal Structure and Properties of a Zinc(Ⅱ) Complex Based on 5-(1H-Tetrazol-5-yl)isophthalic Acid Ligand

A novel polymeric zinc（II） complex {[Zn2（TIA）（H2O）3]·（NO3）}n（1, H3TIA = 5-（1H-tetrazol-5-yl）isophthalic acid） has been synthesized in mixed solvents under solvothermal conditions and characterized by elemental analysis, IR spectroscopy and X-ray single-crystal diffraction. Complex 1 crystallizes in orthorhombic, space group Cmcm with a = 10.4210（6）, b =23.3526（14）, c = 6.9214（4）A, V = 1684.37（17）A^3, Z = 4, C9H4N5O（10）Zn2, Mr = 472.91, Dc = 1.865g/cm^3, F（000） = 932, λ（MoK α） = 2.909 mm^-1, R = 0.0423 and wR = 0.1287. The complex has good thermal stability and excellent photoluminescent property.

Synthesis,Crystal Structure,Theoretical Calculations,and Photoluminescent Property of a Mn(Ⅱ)Complex Assembled by 5-Aminoisophthalic Acid and Phen Ligands

A coordination polymer [Mn2（ctpt）2（aic）2]n （1, ctpt = 2-（4-chloro-phenyl）-1H- 1,3,7,8-tetraaza-cyclopenta[l]phenanthrene, H2aic = 5-amino-isophthalic acid） was hydrother- mally designed and synthesized. The complex was characterized by elemental analysis, IR spectro- scopy, single-crystal X-ray diffraction, and thermogravimetric analysis （TGA）. Each Mn（II） atom is linked by the aic ligands with neighbor Mn（II） atoms, forming an infinite one-dimensional （1D） double-chain structure. Complex 1 crystallizes in monoclinic, space group C2/c, with a = 18.23（1）, b = 17.27（1）, c = 16.69（1） ？, V = 4814.0（7） ？3, C27H16ClMnN5O4, Mr = 564.84, Dc = 1.559 g/cm3, μ（MoKα） = 0.706 mm-1, F（000） = 2296, Z = 8, the final R = 0.0487 and wR = 0.1269 （I 〉 2σ（I））. The 1D chain structure of complex 1 is stable below 458 ℃. In addition, to elucidate the essential electronic characters of this complex, theoretical calculation analysis of 1 was performed by the PBE0/LANL2DZ method in Gaussian 03 Program.

Hydrothermal Synthesis and Crystal Structure of One 3D Coordination Polymer of Nickel(Ⅱ) Achieved from 5-Iodo-isophthalic Acid Ligand

A new coordination polymer [Ni（L）（m-bix）（H2O）]n （1, H2L = 5-iodo-isophthalic acid, m-bix=1,3-bis（imidazol-1-ylmethyl）-benzene） has been synthesized by the hydrothermal method and characterized by IR, elemental analysis, powder XRD and single-crystal X-ray analysis. The crystal is of triclinic, space group Pī with a = 9.1638（3）, b = 10.2319（3）, c = 13.2463（4） ？, α = 80.1710（10）, β = 83.671（2）, γ = 70.3790（10）o,C22H19NiIN4O5, Mr = 605.02, V = 1150.85（6） ？3, Dc = 1.746 g/cm3, F（000） = 600, μ = 2.225 mm-1, S = 1.045 and Z = 2. The final R = 0.0388 and wR = 0.1257 for 5089 observed reflections with I 〉 2σ（I）. In the title complex, the M and P layers are arranged alternately to give a double-layer structure by the symmetry related hydrogen bonds, and these double-layers are further joined together to achieve a 2D supramolecular architecture through I···π interaction involving iodine atoms and imidazole rings. The thermal stability of the title complex was studied by thermal gravimetric （TG） and differential thermal analysis （DTA）.

Syntheses, Structures and Properties of Three Novel La(Ⅲ)/Co(Ⅱ) Coordination Polymers Based on 5-(3-(Tetrazo-5-yl)phenyl)isophthalic Acid

Three novel complexes, namely {[La(tapipa)(4,4′-bibp)·(H2O)2]·H2O}n(1),{[La-(tapipa)(H2O)4(OH)]·3 H2O}n(2),[Co(tapipa)(1,4-bbib)]n(3)(tapipa = 5-(3-(tetrazo-5-yl)phenyl)isophthalic acid, 4,4′-bibp = 4,4′-bis(imidazolyl)biphenyl, and 1,4-bbib = 1,4-bis(benzimidazo-1-ly)benzene) have been synthesized under solvothermal conditions and characterized by PXRD, IR,TGA, and so on. Complex 1 presents a 2 D layer structure, which is finally packed into a 3 D supramolecular structure by means of hydrogen bonds;complexes 2 and 3 exhibit 1 D chains and 2 D wavy-type structures, respectively, which are expanded into 3 D supramolecular structures through hydrogen bonds and π-π interactions. Furthermore, the luminescence properties of complex 1 and the variable-temperature magnetic susceptibilities of 3 were investigated. Complex 1 has highly selective sensing for Fe^3+ and Cr2O7^2- ions.

Synthesis and Crystal Structure of a Two-dimensional Cobalt Complex with 5-Tert-butyl Isophthalic Acid

The self-assembly of Co（OAc）·4H2O with H2tbip and bipy （H2tbip = 5-tert-butyl isophthalic acid, bipy = 4,4＇-bipyridine） generates one new complex, [Co3（tbip）2（Htbip）2（bipy）]n, which has been characterized by elemental analysis, X-ray diffraction, and IR spectroscopy. Single-crystal X-ray analysis reveals that it crystallizes in the triclinic space group P1 with a = 9.471（6）, b = 12.597（8）, c = 12.899（8）, α = 84.660（7）, β = 70.548（7）, γ = 81.965（7）o, V = 1435.1（15）3, Mr = 1215.85, Dc = 1.407 g/cm3, Z = 1, F（000） = 629, μ（MoKα） = 0.926 mm-1, the final R = 0.0623 and wR = 0.1724. The complex consists of a tbip bridged trinuclear cobalt（） unit and is further linked by 4,4＇-bipyridine molecule to form a 2D supramolecular network.

Syntheses and Crystal Structures of Co(Ⅱ)Complexes with 5-Tert-butyl Isophthalic Acid

Two new Co（ Ⅱ） coordination polymers {[Co（Htbip）2（H2O）4]·（H2O）}n 1 and {[Co2（tbip）2Copa）1.5]（H2tbip）}n 2 （H2tbip = 5-tert-butyl isophtha]ic acid, bpa = 1,2-dis（4-pyri- dyl）ethane） have been synthesized under hydrothermal conditions and characterized by elemental analysis, IR spectroscopy and X-ray diffraction. Compound 1 exhibits a water-bridged 1-D linear chain which is extended by hydrogen bonds into a 3D supramolecular network, while compound 2 has a dinuclear unit extended by bpa ligand to form a 2-D layer.

Hydrothermal Synthesis,Crystal Structure and Properties of a Novel 3D Metal-organic Coordination Polymer with Helical Chains Based on 5-(Imidazol-1-ylmethyl)isophthalic Acid

A novel 3D metal-organic coordination polymer with helical chains based on a flexible 5-（imidazol-1-ylmethyl）isophthalic acid（H_2L） as a main ligand and 1,2-bis（4-pyridyl）ethane（bpa） as a N-containing ancillary ligand,[Cd L（bpa）_（0.5）]_n（1）,has been obtained under hydrothermal conditions and characterized by elemental analysis,powder X-ray diffraction（PXRD）,IR,thermal gravimetric analyses（TGA） and single-crystal X-ray diffraction.It crystallizes in monoclinic,space group P2_1/c with a = 10.984（2）,b = 10.1829（12）,c = 17.782（3） A,β = 123.156（11）o,V = 1665.1（5） A^3,Z = 4,Mr = 448.72,Dc = 1.790 g/cm^3,Rint = 0.0871,F（000） = 892,the final R = 0.0687 and w R = 0.1294 for 2920 observed reflections（I 〉 2σ（I））.In complex 1,the L^2- anions connect Cd（Ⅱ） ions to form two-dimensional metal-organic layers（Cd_2L_2）n,in which the 1D helical chains（Cd-L）_n are alternately arranged in a right-and left-handed sequence.These layers are further linked to build a 3D network by the bpa ligand.In addtion,photoluminescent properties for 1 are also investigated.

A Novel 3D Supramolecular Framework of Poly[(5-(oxidediphenylphosphino)isophthalate)zinc(Ⅱ)]: Syntheses and Structure

A novel metal-organic framework, namely [Zn（C20H13OsP）]n （1）, has been hydro- thermally synthesized through the reaction of 5-（oxidediphenylphosphino）isophthalic acid （H2L） with Zn（II） salt. The title compound crystallizes in monoclinic, space group P21/c with a = 11.0966（10）, b = 14.5651（14）, c = 14.7311（15） A, fl = 130.022（6）°, C2oH13OsPZn, Mr = 429.64, V= 1823.3（3） ./k3, Dc = 1.565 g/cm3, F（000） = 872, g = 1.463 mm＂1, S = 1.054 and Z = 4. The final R = 0.0270 and wR = 0.0739 for 2769 observed reflections with 1 〉 20（/）. In the title complex, the Zn2（CO2）2 binuclear clusters are linked by L2- ligands to result in a pillared layer structure in the bc plane, which is a （4,4）-net composed of helical chains with opposite chirality by sharing Zn2（CO2）2 units. Adjacent＇layers are further associated together through Zn-O bonds involving the metal center and the oxygen atom of P=O group to achieve a 3D architecture, in which one-dimensional qua＆angled channel displays the interweaving of two pairs of coaxial double-helical chains with opposite chirality. The luminescence property and thermogravimetric analysis of the title complex were investigated.

A Cu(Ⅱ) Coordination Polymer with 5-Tert-butyl Isophthalate Linker:Synthesis,Crystal Structure,and Magnetic Properties

A new Cu（Ⅱ） metal-organic coordination polymer, {[Cu2（tbip）2（bie）2]·H2O}n （1, H2tbip = 5-tert-butyl isophthalic acid, bie = 1,2-bis（imidazol-1 ＇-yl）ethane）, was assembled under hydrothermal conditions by the reactions of Cu（Ⅱ） acetate with H2tbip and bie. Complex 1 was characterized by elemental analysis, IR spectroscopy and X-ray single-crystal diffraction. Complex 1 crystallizes in triclinic, space group P1, with a = 9.9145（10）, b = 13.2211（13）, c = 15.4363（15） nm, a = 87.0250（10）, β = 88.3220（10）, γ = 83.8240（10）°, V= 2008.4（3） nm3, Z = 2, Dc = 1.505 Mg/m3, F（000） = 944, g = 1.125 mm^-1, S = 1.030, the final R = 0.0336 and wR = 0.0790. The results reveal that complex 1 is a two-dimensional layered structure. In addition, magnetic properties of I were also investigated.

A Co(Ⅱ) Coordinated Polymer with 2-Fold Interpenetration 3D Architecture Based on 5-(Imidazol-1-ylmethyl)isophthalate: Hydrothermal Synthesis, Crystal Structure and Properties

One cobalt coordinated polymer with 2-fold parallel interpenetration 3D architecture based on flexible 5-（imidazol-1-ylmethyl）isophthalate （L2-） as a main ligand and 4,4＇-bipyridine （bpy） as a nitrogen-containing ancillary ligand, {[CoL（bpy）0.5（H2O）3]2}n （1）, has been obtained under hydrothermal conditions and characterized by elemental analysis, powder X-ray diffraction （PXRD）, IR spectra, Uv/vis spectra, thermal gravimetric analyses （TGA） and single-crystal X-ray diffraction. It crystallizes in monoclinic, space group C2/c with a = 26.323（4）, b = 14.696（2）, c = 26.630（4） A, β= 157.747（4）°, V = 3901.2（1） A3, Z = 8, Mr= 435.27, Dc = 1.480 g/cm3, /t= 0.923 mm^-1, Rint = 0.0900, F（000） = 1792, the final R= 0.0722 and wR = 0.0946 for 3641 observed reflections （I 〉 2tr（/））. Complex 1 exhibits a two-fold interpenetration 3D framework. As a single net of the 2-fold interpenetration structure, the L2- anion of complex 1, as a bridging ligand, connects the Co（Ⅱ） ion to form two-dimensional layers （Co3L3）n which are further linked to build a three-dimensional framework by bpy ligand.

The Effect of 19-Substituent on the Stereospecific Hydroxylation of △~5-Steroids Using Performic Acid as Oxidant

In the studying of the stereospecific hydroxylation of different Δ5-steroids with performic acid, followed by hydrolysis with CH3OH/KOH, we found 19-substituting groups considerably affected the reaction and we put forward the mechanism.

间苯二甲酸二甲酯-5-磺酸钠的合成

以w(SO3) =3 0 %的发烟硫酸为磺化剂 ,间苯二甲酸 (IPA)为反应原料制备间苯二甲酸二甲酯 5 磺酸钠(SIPM)。运用正交实验设计 ,确定了最佳磺化反应条件为 :反应温度 185℃ ,反应时间 4 5h ,反应原料配比n(IPA)∶n(SO3) =1 0 0∶1 15。通过高效液色谱 (HPLC)法确定中和深度控制在pH =5 0。SIPM制备收率达到85 2 % ,w(SIPM ) =99 5 % ,各项指标符合美国杜邦公司 2 0 0

5-异烟酰胺基异酞酸与含氮配体构筑的两个铜配合物：水热合成、晶体结构和磁性质研究(英文)

由水热法合成了2个铜配合物[Cu(INAIP)(bbi)].5H2O(1)和[Cu(INAIP)(phen)(H2O)].H2O(2)(H2INAIP=5-异烟酰胺基异酞酸,bbi=1,4-二咪唑基丁烷,phen=1,10-邻菲咯啉),并用元素分析、IR及X-射线单晶衍射等对其进行了表征。晶体结构分析结果表明:配合物1和2都属于单斜晶系,C2/c空间群。配合物1是由1,4-二咪唑基丁烷连接[Cu(INAIP)]一维链形成的二维双层结构,而配合物2是通过π-π堆积作用将[Cu(INAIP)]一维无限链延伸为二维结构,这2个化合物最终均被氢键拓展成三维超分子结构。在1.8～300 K温度范围内测试了配合物1和2的变温磁化率,结果表明配合物1中由羧基桥联的双核铜之间存在弱的反铁磁相互作用,而配合物2表现为顺磁性。

pH控制下3,5-二羧基苯氧乙酸-Cd(Ⅱ)配合物的合成及晶体结构

以3,5-二羧基苯氧乙酸(H3L)为配体与醋酸镉在不同pH条件下获得了2个Cd(Ⅱ)配合物[Cd(H2L)2(H2O)4](1)、[Cd(HL)]n(2),通过红外、X-射线单晶衍射等检测手段对所合成的化合物进行了结构表征。测定结果表明,这2个配合物分别为配位分子和三维配位聚合物,其结构的形成与水热条件的pH值密切相关。该结果对以pH值控制配合物结构提供了研究基础。