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 P1 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).     

Synthesis, Characterization and Properties of Tri-substitute Potassium Salt of Trinitrophloroglucinol

The title complex [K3（TNPG）·（H2O）2]n was synthesized by the reaction of the aqueous solutions of trinitrophlomglucinol （TNPG） with KHCO3. The complex was characterized by elemental analysis and FTIR spectroscopy, and its single crystal structure was determined by X-ray diffraction analysis. The structural analysis demonstrates that two different coordination modes of K cations [K（1） and K（2）] are around TNPG^3- anions in complex [Ka（TNPG）·（H2O）2]n, where the coordination numbers are eight. All K atoms coordinate with O atoms of phenolic hydroxyl group and nitro-group simultaneously. The thermolysis of the [Ka（TNPG） · （H2O）2]n has been investigated by using differential scanning calorimetry （DSC） and thermogravimetry-derivative thermogravimetry （TG-DTG） at a heating rate of 10 ℃/min. The thermal decomposition processes of the title complex were comprised of one endothermic dehydration stage and one exothermic decomposition stage in 270-320℃, and the final decomposition residue contained KNC. Impact and friction sensitivity results of the complex revealed its sensitive nature towards mechanical stimuli. The experiments verified that the complex has some characteristics of explosive.     

Synthesis,Crystal Structure and Biological Activity of 1-（β-D-Glucopyranosyl）-3- amino-5-methyl-1H-1,2,4-triazole

The title compound 1-（β-D-glucopyranosyl）-3-amino-5-methyl- 1H- 1,2,4-triazole was synthesized and characterized by IR, 1H-NMR and elemental analysis. Its single crystals of 2H2O adduct suitable for X-ray analysis were obtained by the slow evaporation of a H2O solution and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to orthorhombic, space group P212121 with a = 7.7490（15）, b = 10.424（2）, c = 17.447（4） A^°, V = 1409.3（5） A^°^3, Z= 4, C9H20N4O7, Mr = 296.29, Dc = 1.396 g/cm^3,μ = 0.120 mm^-1, S = 1.007, F（000） = 632, R = 0.0686 and wR = 0.1560 for 1217 observed reflections with I 〉 20（I）. The title molecules are linked through intermolecular hydrogen bonds to form two 1-D chain structures, and such adjacent chains are further linked by intermolecular hydrogen bonds and H2O bridges to form a 3-D supramolecular network structure. The preliminary bioassay results showed that the title compound exhibits fungicidal activities against Gibberella zeae and Colletotrichum orbiculare.     

Syntheses,Crystal Structures and Intermolecular Interactions of Cu（II） Complexes with Methyl- benzoic Acid （MBA） and 1,10-Phenanthroline

Two cupric complexes containing methylbenzoic acid have been prepared and crystallized by solvent evaporation method in DMF. The single-crystal X-ray crystallographic analysis reveals that they are dicaryon complexes. Complex I with formula of [Cu2（m- MBA）4DMF2] crystallizes in monoclinic with space group of P21/c and complex 2 with formula of [Cuz（o-MBA）ffo-phen）2]·NO3·H2O crystallizes in triclinic with space group of P I. The weak interactions including C-H...O hydrogen bonds, C-H…π interactions and π-π stacking in the structures of two complexes are observed from the X-ray crystallographic data. In addition, there are still classical hydrogen bonds in 2. The different strength of intermolecular interaction in the structure is reflected on their different thermal stability measured by thermal gravimetric analysis and 2D-1R correlation spectroscopy of two complexes. The study of weak interactions is meaningful to provide supporting data for supramolecular chemistry theory and potential applications in molecular biology.     

Antitumor Metallothiosemicarbazonate： Synthesis,Crystal Structure,Spectra and Antitumor Studies of Co（Ⅲ） Complex with Thiosemicarbazone Derivative of 2-Benzoylpyridine

The title complex [Co（L）2]Cl·4H2O I has been achieved via self-assembly by incorporating cobalt into 2-benzoylpyridine thiosemicarbazonate ligand, and characterized by elemental analysis, infrared spectra, mass spectra and single-crystal X-ray diffraction study. The crystal crystallizes in monoclinic, space group P2 1/n, with a = 10.227（3）, b = 17.363（4）, c = 17.459（4） A, β= 100.408（4）°, V= 3049.2（13） A^3, Z = 4, Mr = 677.08, Dc = 1.475 g/cm^3, μ（MoKα） = 0.834 mm^-1, F（000） = 1400, the final R = 0.0747 and wR = 0.0896 for 1663 observed reflections with I 〉 2σ（I）. The complex contains one six-coordinated cobalt ion connected by two thiosemicarbazone ligands which act as a tridentate ligand to coordinate with the center metal atoms via two pyridyl nitrogen atoms, two imine nitrogen atoms and two sulfur atoms giving rise to a mononuclear structure. Hydrogen bonds existing in the complex link the different components to stabilize the crystal structure. The antiturnor activity of the title complex was tested against A549 lung cancer cell line. Complex ! exhibits antitumor activity.     

Hydrothermal Synthesis and Crystal Structure of a Novel Binuclear Cd（ Ⅱ ） Coordination Polymer Based on 1,2-Benzenedicarboxylate and Imidazole

The hydrothermal reaction of Cd（OAc）2.H2O with 1,2-benzenedicarboxylate （1,2-BDC）, imidazole and H2O resulted in the formation of a binuclear polymeric Cd（ Ⅱ ） complex {[Cd2（1,2-BDC）2（Im）4].（H2O）}n which was then characterized by elemental analyses and single-crystal X-ray diffraction analysis. The crystal is of monoclinic system, space group P21/c with a = 14.6455（3）, b = 9.3530（2）, c = 23.7838（5）A, β= 106.6290（10）°, Cl12H104CdgN32O36, Mr = 3373.47, V = 3121.64（11）A^3, Dc = 1.795 g/cm^3, F（000） = 1672,μ= 1.428 cm^-1 and Z = 1. The final R = 0.0316 and wR = 0.0687 for 5045 reflections with I 〉 2σ（I）. In the title complex, the two Cd（ Ⅱ） ions are in different coordination environments with distorted octahedral and pengonal bipyramidal geometries, respectively. Two Cd polyhedra are linked together through one μ2-η^1：η^1 and one μ2-η^1：η^1 carboxylate groups from different 1,2-BDC ligands, giving rise to a binuclear Cd（ Ⅱ ） cluster, and such clusters are connected by bridged 1,2-BDC ligands to form a 2-D structure along the c axis. The inter- and intermolecular hydrogen bonds further connect the 2-D structures into a 3-D supramolecular network.     

Synthesis and Crystal Structure of a Zeolite-like Metal-organic Framework Based on the Triazole Ligand

A novel zeolite-like metal-organic framework, [Cd12（trz）12＇F10＇（SiF6）3]·（H3O）4 （Htrz = 1,2,4-triazole）, has been synthesized under solvothermal conditions using 1H-l,2,4-triazole-3- carboxylic acid and CdF2 as the starting materials. The complex has been characterized by elemental analysis, IR, SEM-EDS, gas adsorption, powder and single-crystal X-ray diffraction analyses. The title complex crystallizes in the cubic 1-43m space group, with a = 14.6436（8）, V= 3140.1（3）A3, Z = 2, Mr = 2857.96, D,.= 3.023 g/cm3 and F（000） = 2668. The final R = 0.0653 and wR = 0.1880 for 586 observed reflections with 1 〉 2σ（I）. In the title complex, three adjacent Cd（ll） centers are connected by three p3-bridging triazole ligands to form triagonal secondary building units （SBUs）, which are further interconnected to form a three-dimensional skeleton with tetrahedral cages.     

Synthesis and Crystal Structure of a Co（ Ⅱ ） Complex with Taurine-5-methyl-2-hydroxyisophthalaldehyde Schiff Bases [Co（C13H16N2O7S2）（H2O）3]2·H2O

The title complex [CoL（H20）3]2·H2O （C26H46N4O21S4CO2）, where L = taurine-5- methyl-2-hydroxyisophthalaldehydes, has been synthesized and characterized by IR and X-ray diffraction analysis. The crystal of the complex belongs to the triclinic system, space group P1, with a = 11.197（4）, b = 13.309（5）, c = 14.486（5） ]A, a = 78.827（13）,β = 70.547（11）, γ = 81.058（13）°, Mr = 996.77, S = 1.08, V= 1987.2（13） A3, Z = 2, Dc = 1.666 g/cm3, F（000） = 1032,μ = 1.131 mm^-1, R = 0.0633 and wR = 0.1293. According to the structural analysis, the Co（ Ⅱ ） ion adopts a slightly distorted six-coordinated octahedral geometry. One N atom of the Schiff base of each molecule was hydrogenated to form hydrogen bond with O atom. Two coterminous molecules packed in one crystal water molecule are linked by intermolecular hydrogen bonds, thus generating an infinite chain constructed by hydrogen bonds.     

Synthesis, Crystal Structure and Thermal Stability of a Saturated Dimeric Ce（III）-chelated Complex Based on Benzoate and 1,10-Phenanthroline Ligands

The title complex, [Ce（BA）3phen]2 （BA = benzoate, phen = 1,10-phenanthroline）, was prepared by the reaction of Ce（NO3）3.6H2O, benzoic acid and 1,10-phenanthroline. The complex was characterized by single-crystal X-ray diffraction, elemental analysis, IR spectra and TG-DTG techniques. The results show that the crystal is of triclinic, space group P1 with a = 10.912（2）, b = 11.962（3）, c = 12.474（3） A, α = 104.889（3）, β = 93.523（3）, γ = 113.332（3）^o, C66H46Ce2N4O12, Mr = 1366.90, V= 1420.2（6） ,A^3, Z = 1, Dc = 1.598 g/cm^3, μ = 1.652 mm^-1, S = 1.024 and F（000） = 682. The final R = 0.0391 and wR = 0.0947 for 4878 observed reflections with I 〉 2σ（I）. The structure of the title complex consists of two Ce（C6HsCOO）3（C12H8N2） units, forming a binuclear molecule. Each Ce（Ⅲ） is coordinated by two O atoms of one bidentate chelating carboxylate group, five O atoms of two bidentate bridging and two tridentate chelating-bridging carboxylate groups, and two N atoms of one 1,10-phenanthroline molecule to complete a distorted monocapped square antiprism geometry. Its thermogravimetric analysis was determined by TG-DTG techniques.     

Synthesis and Crystal Structure of a Novel Heterometallic Complex [Na2Cu2Gd2（pdc）4（H2O）14·2H2O]

A novel heterometallic complex [Na2Cu2Gd2（pdc）4（H2O）14·2H2O] （H3pdc = 1H- pyrazole-3,5-dicarboxylic acid） has been synthesized and characterized by 1R spectra, elemental analysis, and single-crystal X-ray analysis. The crystal belongs to the monoclinic system, space group P2 1/c with a = 7.9521（18）, b = 12.251（3）, c = 22.293（5） A, β = 110.173（5）°, V= 2038.5（8） A^3, Mr = 1388.13, Z = 2, F（000） = 1352, Dc = 2.261 g/cm^3,/2 = 4.380 mm^-1, the final R = 0.0409 and wR = 0.0622 for 2453 observed reflections with I 〉 2σ（I）. The structural analysis shows that the Na^I, Cu^II and Gd^II ions are linked together by two kinds of bridging ligands （pdc^3- and H2O） to form a main moiety [Na2Cu2Gd2（pdc）4（H2O）14], which can be regarded as a centrosymmetric dimmer of [NaCuGd（pdc）2（H2O）7]. Many hydrogen bonds exist in the complex to build a 3D supramolecular framework.     

Crystal Structure and Polymerization Activity of Bromo-（2-diphenylphosphino-N-（2-oxybenzylidene）-aniline）-nickel

The title compound,bromo-（2-diphenylphosphino-N-（2-oxybenzylidene）-aniline）- nickel,was synthesized by simple condensation of 2-diphenylphosphino-N-（2-oxybenzylidene）- aniline with NiBr2·6H2O and characterized by elemental analysis,IR spectra and single-crystal X-ray diffraction. The crystal belongs to the triclinic system,space group P1 with a = 9.756（2）,b = 10.232（2）,c = 13.313（3）A,α = 95.09（3）,β = 102.48（3）,γ = 95.45（3）o,V = 1283.5（4） A^3,C29H23BrNNiO2P,Mr = 587.07,Z = 2,Dc = 1.519 g/cm^3,λ（MoKα） = 0.71073 A,F（000） = 596 and μ = 2.402 mm^-1. The structure was refined to the final R = 0.0408 and wR = 0.0965 for 4507 observed reflections （I 〉 2σ（I））. Intermolecular π-π interactions （with distances of about 3.705 A） are pronounced in the crystal structure. Under methylaluminoxane （MAO） activation,the title compound was able to catalyze norbornene polymerization,exhibiting good polymerization activities.     

Synthesis,Structure and Properties of a New Lead(Ⅱ) Complex of 1,3-Benzenedicarboxylic Acid, 1,10-Phenanthroline and Its Thermal Decomposition to PbO Micro-crystal Particles

The self-assembly of 1,10-phenanthroline(phen) and 1,3-benzenedicarboxylic acid(H2bdc) with Pb(NO3)2 under solvothermal conditions in N,N-dimethylacetamide(DMA) gives rise to a one-dimensional chain coordination polymer, [Pb(phen)(bdc)](1), which was characterized by elemental analysis, FT-IR and single-crystal X-ray diffraction. This complex crystallizes in triclinic, space group P1 with a = 7.5595(6), b = 9.8199(8), c = 13.1663(11) , α = 69.7590(10), β = 80.6000(10), γ = 71.3180(10)o, Z = 2, C20H12N2O4Pb, Mr = 551.51, Dc = 2.112 g/cm3, F(000) = 520 and μ = 9.757 mm-1. The final R = 0.0304 and wR = 0.0763 for 3427 observed reflections with I 2σ(I) and R = 0.0365 and wR = 0.0894 for all data. The structure contains one crystallographic unique Pb(Ⅱ) atom, one phen molecule chelating with a Pb(Ⅱ) atom, and one bdc2- anion, acting as a bidentate bridging ligand linking the Pb(Ⅱ) atoms to form a one-dimensional structure. The two-dimensional layer and three-dimensional stacking structures are formed by C–H···O hydrogen bonding interactions. The thermal stable and fluorescent properties of 1 were investigated. PbO micro-crystal particles are produced by calcination of powder sample of complex 1. The obtained PbO is characterized and observed by XRD and SEM analyses.     

Crystal Structure and Properties of a Copper(Ⅱ) Complex Containing p-Toluenesulfonate and Imidazole Ligands

A novel supramolecular mixed ligand complex of formula [Cu(PTS)2(Him)2(H2O)2] (C20H26CuN4O8S2,PTS=p-toluenesulfonate,Him=imidazole) has been synthesized in aqueous solution and characterized by elemental analysis,IR and single-crystal X-ray diffraction.The compound crystallizes in the monoclinic system,space group P21/n,Z=2,a=5.650(2),b=14.671(3),c=14.638(3),β=100.10(3)°,V=1194.60(4)3,Dc=1.607 g/cm3,μ(MoKα)=1.143 mm-1,F(000)=598,R=0.0615 and wR=0.1503 for 1752 observed reflections with I 2σ(I).The copper(II) ion in the complex adopts a slightly distorted octahedral coordination geometry and is six-coordinated with N2O4 donor set consisting of two nitrogen atoms and four oxygen atoms provided by the ligands of two imidazole molecules,two water molecules and two p-toluenesulfonate ions.The sulfonate group of the PTS ligand remains weak-coordinated and forms a number of hydrogen bonds with water molecules and imidazole ligands.X-ray structural analysis reveals that the coordination molecules are connected to form a 3-D supramolecular framework by electrostatic interaction,weak van der Waals forces,hydrogen bonding and π-π interaction.The thermal behaviour of the title complex was investigated by using DSC and TG-DTG techniques.     

Hydrothermal Synthesis and Crystal Structure of One 3D Coordination Polymer of Cobalt(II) Achieved from 1,1′-Biphenyl-2,2′,6,6′-tetracarboxylic Acid Ligand

<正>A new three-dimensional coordination polymer {[Co(BPTC)_(0.5)(bix)]·(H_2O)}_n (1, H4BPTC = 1,1′-biphenyl-2,2′,6,6′-tetracarboxylic acid, bix = 1,3-bis(imidazol-1-ylmethyl)-benzene) has been synthesized by the hydrothermal method and characterized by IR, elemental analysis, and single-crystal X-ray analysis. The crystal is of orthorhombic, space group Pbcn with a = 13.2975(10), b = 13.8424(12), c = 22.6367(17), CoC_(22)H_(19)N_4O_5, M_r = 478.34, V = 4166.7(6) ~3, D_c = 1.525 g/cm~3, F(000) = 1968, μ = 0.867 mm~(-1), S = 1.023 and Z = 8. The final R = 0.0683 and wR = 0.1529 for 3655 observed reflections with I > 2σ(I). In the title complex, the 2D Co-BPTC layer is formed through self-assembly of Co(II) ions and bridging BPTC~(4-) ligands in a molar ratio of 2:1. The metal-organic lattice layers are further united together through the second bridging ligand bix to form a 3D metal-organic framework. The thermal stability of the title complex was studied by thermal gravimetric (TG) and differential thermal analysis (DTA).     

Synthesis,Crystal Structure and Thermal Properties of N,N＇-Bis（5,5-dimethyl- 2-phospha-2-thio-1,3-dioxan-2-yl） Ethylene Diamine

The title compound N,N＇-bis（5,5-dimethyl-2-phospha-2-thio-1,3-dioxan-2-yl） ethylene diamine （DPTDEDA, C12H26N2O4P2S2） was synthesized by the reaction of neopentyl glycol, phosphorus thio-chloride and 1,2-ethylenediamine, and characterized by elemental analysis, IR and ^1H NMR spectra. Its crystal structure was determined by single-crystal X-ray diffraction analysis and the thermal property was analyzed by TG analysis. The crystal structure belongs to monoclinic, space group P21/c, with a = 14.557（16）, b = 11.299（12）, c = 12.163（13）A,β = 98.707（19）^o, Dc = 1.305 g/cm^3, Z = 4, γ = 0.71073A,μ（MoKa） = 0.447 mm^-1, Mr = 388.41, V = 1977（4）A3, F（000） = 824, S = 1.107, the final R = 0.0478 and wR = 0.0810 for 1738 observed reflections （I 〉 2σ（I））. X-ray analysis reveals that the crystal structure is centrosymmetrically distributed through 1,2-ethylenediamine to join two distorted six-membered rings. The weak N-H…S interactions are observed and link the molecules into sheets. TG analysis shows that the title compound has good thermal stability and char-forming capability, which are required for an excellent intumescent fire retardant.     

Preparation, Crystal Structure, and Thermal Analysis of Carbohydrazide Trinitrophloroglucinolate

A new compound （CHZ）（HTNPG）·0.5H2O was synthesized by mixing carbohydrazide（CHZ） and trinitrophloroglucinol（TNPG） and characterized by elemental analysis and Fourier transform infrared （FTIR） spectrum. Its crystal structure was determined by single crystal X-ray diffraction analysis. The crystal belongs to triclinic system, P1 space group, with a=0.45578（9） nm, b=1.0142（2） nm, c=1.3041（3） nm, α=86.53（3）°, β=99.56（3）°, γ=81.94（3）°, V= 0.5958（2） nm^3, Z=2, Dc=2.008 g/cm^3, R1=0.0476, and wR2=0.1139. The compound is a di-substituted salt of TNPG, which consists of a cation （CHZ）^2＋ and an anion （HTNPG）^2-. The thermal analysis of the compound was studied by means of differential scanning calorimetry（DSC） and thermogravimetry-derivative thermogravimetry（TG-DTG）. Under nitrogen atmosphere at a heating rate of 10 ℃/min, the thermal decomposition of the compound contained one endothermic process of dehydrating stage and two intense exothermic decomposition processes in a temperature range of 140--232 ℃ on the DSC trace. The decomposition products of the title compound are nearly gaseous products. The existing complicated hydrogen bond networks and electrostatic attraction between （CHZ）^2＋ and （HTNPG）^2- enhance the thermal stability of the title compound.     

Hydrothermal Synthesis and Characterization of a Two-dimensional Layer Based on Keggin POM Cluster Units： [Cu2（DMPz）2PMo12O40]＇HDMPz

The title compound, [Cu2（DMPz）2PMo12O40]·HDMPz （1, DMPz = 2,5-dimethyl pyrazine）, has been synthesized and characterized by single-crystal X-ray diffraction analysis. It crystallizes in triclinic, space group P1 with a = 11.075（2）, b = 11.551（2）, c = 11.886（2） A.α = 106.352（2）, β = 109.862（3）, γ = 109.504（1）°, V = 1206.8（3） A3, C18H26CU2Mo12N6O40P, Mr = 2275.78, Z = 1, Dc = 3.131 g/cm3, μ = 4.011 mm^-1, F（000） = 1073, S = 1.066, the final R = 0.0389 and wR = 0.1056 for 3739 observed reflections with I 〉 2σ（I）. The structural analysis indicates that the title compound is composed of Keggin clusters [PMo12O40]3- connected by one-dimensional [CB（DMPz）]2n^2n＋ chains to form a two-dimensional grid layer with holes occupied by monoprotonated DMPz molecules. In the solid of the title compound, the 2D grid layers are stacked together in an ABAB packing mode.     

Synthesis and Crystal Structure of 5,17-Diformyl-11,23-di（tert-butyl）25,26,27,28-tetrapropoxy-calix[4]arene

The title compound 5,17-diformyl-11,23-di（tert-butyl）-25,26,27,28-tetrapropoxycalix[4]arene has been synthesized by selective formylation of 5,11,17,23-tetra（tert-butyl）25,26,27,28-tetrahydroxycalix[4]arene in three steps and characterized by1H NMR and X-ray single-crystal diffraction.The crystal belongs to the monoclinic system,space group C2/c with a = 25.760（3）,b = 10.9952（10）,c = 18.630（2）,β = 119.985（4）°,V = 4570.4（9）3,Z = 4,Dc = 1.106 g/cm3,Mr = 761.01,F（000） = 1648,μ = 0.071 mm-1,MoKa radiation（λ = 0.71073）,R = 0.0710 and wR = 0.2411 for 3234 observed reflections with I 2σ（I）.X-ray analysis reveals that the title compound adopts a pinched cone conformation which leads to an open cavity.Intermolecular C–H O weak interactions link the molecules along the bc plane,which are effective in the stabilization of the crystal structure.     

Synthesis,Structure and Photoluminescence of a Binuclear Zinc（Ⅱ） Coordination Polymer Based on 2-Carboxycinnamic Acid and Dipyrido [3,2-a： 2＇,3 ＇-c]-phenazine

A binuclear zinc（Ⅱ） complex with 2-carboxycinnamic acid （2-ccm） and dipyrido- [3,2-a：2＇,3＇-c]phenazine （DPPZ）, {[Zn2（2-ccm）2（DPPZ）2]·2H2O}n, was synthesized and characterized by elemental analysis, IR, single-crystal X-ray diffraction, thermal gravimetry and fluo- rescent emission. It crystallizes in monoclinic, space group P21/c with a = 13.409（4）, b = 25.530（7）, c = 13.952（4） A, β = 99.554（3）°, V= 4710（2） A3, Z= 4, C56H36N8O10Zn2, Mr= 1111.67, Dc = 1.568 g/cm3, μ（MoKα） = 1.093 mm^-1, F（000） = 2272, R = 0.0422 and wR = 0.0895. In the crystal, the basic unit of 1 is a binuclear Zn2 entity which is linked by 2-ccm ligand to form a 1D double chain along the a axis. The O-H...O hydrogen bonding and π-π interactions lead to a 3D supramolecular motif. In addition, thermal and luminescent properties of complex 1 have also been investigated.     

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

A novel metal-organic framework, namely [Zn(C20H13O5P)]n(1), has been hydrothermally 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), β = 130.022(6)o, C20H13O5 PZn, Mr = 429.64, V = 1823.3(3) 3, Dc = 1.565 g/cm3, F(000) = 872, μ = 1.463 mm-1, S = 1.054 and Z = 4. The final R = 0.0270 and wR = 0.0739 for 2769 observed reflections with I 2σ(I). 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 quadrangled 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.