6,8-Di-tert-butyl-3-(2,4-dimethyl-quinolin-7-yl)-3,4-dihydro-2H-benzo[e][1,3]oxazine: Synthesis, Crystal Structure and Luminescent Properties

6,8-Di-tert-butyl-3-（2,4-dimethyl-quinolin-7-yl）-3,4-dihydro-2H-benzo[e][1,3]oxa- zine（1） was obtained by one-pot reaction starting from 2,4-di-tert-butylphenol, 7-amino-2,4- dimethyl-quinoline and paraformaldehyde. The compound was structurally characterized by NMR, IR and single-crystal X-ray diffraction along with the elemental analysis. Compound 1 crystallizes as solvate with chloroform. The solvate 1·CHCl3（C28 H35 Cl3 N2 O, Mr = 521.93） belongs to the triclinic system, space group P1 with a = 10.852（2）, b = 11.352（2）, c = 13.050（3）, α = 101.95（3）, β = 92.94（3）, γ = 114.64（3）o, V = 1412.4（5）3, Z = 2, Dc = 1.227 g/cm3, F（000） = 552, μ = 0.347 mm–1, R = 0.0959 and wR = 0.2725（I 〉 2？（I））. The chloroform molecule displays a rotational disorder as one chloro atom can be located at two different positions. The packing of 1·CHCl3 was further stabilized by intramolecular C–H…O interactions, intermolecular C–H…N interactions, C–H…π interactions, and π…nteractions. The luminescent properties of compound 1 in both methylene chloride solution and the solid state were studied.

Synthesis, Crystal Structure and Luminescent Properties of a Novel 1D Zigzag Chain Barium(Ⅱ) Coordination Polymer

A new coordination polymer {[Ba（L）（H2o）5]·H2O}n （1, H2L = 3,3＇-（（（（ethane-l,2- diylbis（oxy））-bis（2,1-phenylene））bis（methylene））bis（oxy））dibenzoic acid） has been synthesized under evaporation process and characterized by elemental analysis, IR spectra, TG analysis, fluorescence spectrum, powder X-ray diffraction analysis and single-crystal X-ray diffraction. Complex 1 crystallizes in the monoclinic system, space group P21/c, with a = 20.918（5）, b = 7.4539（2）, c = 20.168（5）A, β = 95.486（2）°, V= 3130.1（1） A.3, Z= 4, C30Ha4BaO14, Mr = 755.91, Dc = 1.604 g/cm3, F（000） = 1528,μ = 1.34 mm-1, the final R = 0.0404 and wR = 0.0676 for all data. Single-crystal X-ray structural reveals that the Ba（II） ion adopts a nine-coordinated distorted tricapped trigonal prism coordination geometry. Adjacent Ba（lI） ions are linked by one μ2-L2- anion and two （μ2-H20） water molecules to generate an infinite 1D zigzag chain structure. Then these chains are further linked into a 2D layer supramolecular architecture through O-H…-O hydrogen bonds. Luminescent property and thermal stability of complex I were investigated.

Synthesis,Crystal Structure and Luminescent Properties of a 1D Loop-chain Coordination Polymer [Ag(3,3-pybz)(3,3-Hpybz)]_n

A new coordination polymer, [Ag（3,3-pybz）（3,3-Hpybz）]n （1, 3,3-Hpybz = 3-pyri- din-3-yl-benzoic acid）, has been synthesized and characterized by elemental analysis, IR spectra, PXRD, and single-crystal X-ray diffraction. In complex 1, the Ag（1）ions are linked by the paired 3,3-pybz ligands to generate an infinite 1D loop chain, and further through π-π stacking interactions to form a 2D supramolecular architecture. Crystal data for 1： triclinic, space group P1, a = 10.2635（17）, b = 10.3041（12）, c = 10.8060（13） A, V= 1679.1（5）A3, α = 62.028（11）, β = 80.325（15）, γ = 78.738（14）°, Z = 2, C24H17AgN2O4, Mr = 505.27, Dc= 1.698 g/cm3, μ= 1.058 mm--, F（000） = 506, S = 1.012 and T = 293（2） K. The final R = 0.0293 and wR = 0.0667 for 3435 observed reflections with I〉 2a（/）, and R = 0.0350 and wR = 0.0688 for all data.

Synthesis,Crystal Structure and Luminescent Properties of a Novel Zinc(II) Complex of N-Acetyl-L-glutamic Acid and Imidazole Ligands

A novel complex [Zn（Im）2（A-glu）]-0.5H2O（Im = imidazole, A-glu = N-acetyi- L-glutamic acid） has been synthesized from the reaction of A-glu with Zn（CH3COO）2·2H20 in the presence of Im at 65 ℃, and structurally characterized by single-crystal X-ray diffraction. The complex crystallizes in tetragonai, space group P43212 with a = b = 8.9078（6）, c = 43.458（6） A, C26H36N10O11Zn2, Mr = 795.39, V= 3448.3（6） A^3, De = 1.532 g/cm^3, Z = 4,μ（MoKα） = 1.461 mm^-1, F（000） = 1640, the final R = 0.0453 and wR = 0.0992. X-ray analysis reveals that the crystal structure is constructed by mixed iigands. A-glu adopts the bis-monodentate coordination mode linking two adjacent metal ions to form a one-dimensional chain. Zinc（Ⅱ） ions are four-coordinated with a distorted tetrahedral geometry. Luminescent properties of the complex have been inves- tigated.

Crystal Structure and Luminescent Properties of a Zn(Ⅱ) Coordination Polymer Assembled by Mixed-ligand

A Zn（Ⅱ） coordination polymer [Zn（NIP）（3,3＇-bpt）].H20 （1, NIP = 5-nitroisophtha- late, 3,3＂-bpt = 1H-3,5-bis（3-pyridyl）-l,2,4-triazolate） has been synthesized by the hydrothermal reaction at 140 ℃ and structurally characterized by IR spectroscopy, X-ray diffraction, thermal analysis, single-crystal X-ray diffraction and luminescent properties. In complex 1, the zinc atom is five-coordinated with three carboxylate oxygen atoms from three H2NIP and two nitrogen atoms from two 3,3＇-bpt, respectively, forming a distorted trigonal bipyramidal geometry and showing a 1D chain structure, which is further bridged by NIP to form a 3D supramolecular network via self-assembly of hydrogen bonds.

Crystal Structure and Luminescent Properties of[Cu(phen)_2I][Bi(phen)I_4]

The title complex, [Cu（phen）2I][Bi（phen）I4], has been successfully synthesized by a solution method. Its crystal structure was determined by X-ray diffraction method, and crystallizes in triclinic, space group P1 with a = 10.3876（2）, b = 14.4258（5）, c = 14.7128（5） ？, α = 82.569（8）, β = 73.442（7）, γ = 79.299（8）°, V = 2069.68（11）A3, Z = 2, Dc = 2.323 g/cm3, F（000） = 1318, μ（Mo Kα） = 13.132 mm–1 and T = 293（2） K. The final R = 0.0472 and w R = 0.1147 for 6027 observed reflections with I 〉 2σ（I）. In the structure of the title compound, [Bi（phen）I4]– provides us an opportunity to survey the influence of coordination component on the structure of the cation in the [Cu（phen）2I][Y] system. X-ray diffraction and luminescent spectrum study of the complex are also described.

Synthesis,Crystal Structure and Luminescent Properties of [Ag(bzdmpymt)]_6·2MeOH(bzdmpymtH = 5-Benzyl-4,6-dimethylpyrimidine-2-thione)

Reaction of AgAc with bzdmpymtH in MeOH resulted in the title compound [Ag（bzdmpymt）]6-2MeOH （1.2MeOH）, which was structurally characterized by elemental analysis, IR, and single-crystal X-ray diffraction analysis. 1.2MeOH belongs to the triclinic system, space group Pi, with a = 10.930（2）, b = 11.646（2）, c = 16.794（3）A, a = 103.97（3）, β = 97.07（3）, γ = 97.94（3）°, V = 2027.2（7） A3, Z = 1, μ = 1.629 mm^-1, Dc = 1.710 mg/m3, T = 193（2） K, CsoH86Ag6N12O2S6, Mr = 2087.25, F（000） = 1044, S = 1.034, R = 0.0355 and wR = 0.0709. In 1.2MeOH, six silver（I） atoms are held together by six bzdmpymt ligands through N and S atoms to form a water-wheel-shaped structure. Each Ag atom is coordinated by two S atoms from two bzdmpymt ligands and one N atom from the third bzdmpymt ligand, giving a trigonal planar coordination geometry. Interactions between the CH3 group of bzdmpymt ligand and one pyrimidyl nitrogen atom in an adjacent molecule afford a one-dimensional hydrogen-bonding chain running along the b axis. The luminescent property of 1.2MeOH was also investigated.

Syntheses,Crystal Structures and Luminescent Properties of Three New Gallium Complexes Containing Pyridine-2,6-dicarboxylic Acid

Three new gallium complexes formulated as [Ga（PDA）2 ][Ga（H2O）（PDA）（phen）]·4H2O（1）,[Ga（PDA） 2]·（H2IN）·2H2O（2） and [Ga（OH）（PDA）（H2O）] 2（3）（H2PDA=pyridine-2,6-dicarboxylic acid;phen=1,10-phenanthroline;HIN=isonicotinic acid） have been synthesized under hydrothermal conditions.In the mixed-ligand system of complex 1,PDA2 and phen are connected to the central Ga 3＋ cation as tri-and bi-dentate ligands,respectively.In complex 2,each Ga 3＋ cation is six-coordinated by two PDA 2 anions octahedrally.Complex 3 shows a binuclear structure,with the bond distance of Ga1― Ga2 being 0.30061（3） nm.The 3D supramolecular structures of the three complexes are constructed via hydrogen bonds and aromatic π-π packing interactions.All the three complexes exhibit intense blue emission at room temperature in the solid state,which are attributed to π＊-π transition centered on the ligands.

Synthesis,Structure and Luminescent Properties of [Zn(btzb)_2Cl_2]·2H_2O [btzb=1,2-Bis(5-tetrazolyl)benzene]

The title compound [Zn（btzb）2Cl2]·2H2O （1·2H2O, btzb = 1,2-bis（5-tetrazolyl）ben- zene） was synthesized in situ by the [2＋3] cycloaddition reaction of phthalonitrile with NaN3 in water in the presence of ZnCl2 under refluxing conditions. 1·2H2O crystallizes in the monoclinic system, space group P2 1/c with a = 9.0119（18）, b = 7.5566（15）, c = 18.076（5）A, β= 114.67（2）°, V= 1118.6（4）A^3, Z = 2, Dc = 1.784 g/cm^3, T= 223（2） K, C16H16N16O2Cl2Zn, Mr = 600.74, F（000） = 608, μ（MoKα） = 1.393 mm^-1, S = 1.081, R = 0.0306 and wR = 0.0669 for 1896 observed reflections with I 〉 2σ（I）. The Zn^2＋ ion of 1 is coordinated by four N atoms from two btzb ligands and two Cl atoms, forming a distorted octahedral coordination geometry. A number of intermolecular hydrogen bon- ding interactions between molecules 1 and/or the solvated water molecules result in a 3D hydrogen-bonded structure. The luminescent property of 1·2H2O was also investigated.

Hydrothermal Syntheses, Crystal Structures and Luminescence Properties of Cu(Ⅱ) and Cd(Ⅱ) Complexes Assembled by 6-Hydroxypicolinic Acid and 1,10-Phenanthroline

Two new complexes based on 6-hydroxypicolinic acid(H_2picO) and 1,10-phenanthroline(phen), such as [Cu_4(picO)_4(phen)_4]·12 H_2O(1) and {[Cd_4(picO)_4(phen)_4(H_2O)_2]·5H_2O}_n(2), have been synthesized and characterized by IR, elemental analyses, thermogravimetric analyses and X-ray diffraction technique. Single-crystal X-ray diffraction analyses revealed that the two complexes both crystallize in the triclinic system, space group P(16)-. For complex 1, the picO ligands adopt a tridentate coordination mode to link copper(Ⅱ) ions into dimmers. PicO ligands also adopt a tridentate mode in complex 2, which connects the cadmium(Ⅱ) to form a one-dimensional chain. Moreover, luminescent properties of 1 and 2 were also investigated.

Hydrothermal Synthesis, Crystal Structure and Luminescence Properties of a New 2D Cadmium Complex Based on the 4,4'-Bis(benzimidazol-1-ylmethy1)biphenyl and Glutaric Acid Ligands

A new polymeric complex {[Cd2（bbmb）2（gt）2]＇（H2O）2}, （bbmb = 4,4＇-bis（benzimidazol-l-ylmethyl）biphenyl, H2gt = glutaric acid） has been obtained by hyclrothermal method and structurally characterized by elemental analysis, IR, XRD, TGA and single-crystal X-ray diffraction. The complex belongs to the triclinic system, space group P1 with a = 10.2417（15）, b = 13.752（2）, c = 22.201（3） A, a = 73.899（2）, β = 88.416（2）, y = 78.305（2）°, V = 2940.4（7） A3, Z = 2, C66H56Cd2N808, Mr = 1313.99, Dc = 1.484 g/cm3, F（000） = 1336 and μ = 0.787 mm-1, and features a 2D network. In the solid state at room temperature, the cadmium（Ⅱ） complex exhibits strong fluorescence absorption at 435 nm （λmax）.

Two Interpenetrated and Polycatenated Zn(Ⅱ)Coordination Polymers:Syntheses,Structures and Luminescent Properties

Two fascinating Zn（II）entangled coordination polymers,[Zn（eoba）(bbi)];·nH;O（1）and[Zn（boba）(bbi);];（2）,(bbi=1,1?-（1,4-butanediyl）-bis（imidazole）,H;eoba=4,4?-（ethane-1,2-diyldioxy）-dibenzoic acid,H;boba=4,4?-（butane-1,4-diyldioxy）-dibenzoic acid),were obtained by hydrothermal technology and characterized by elemental analysis,infrared spectrum,thermogravimetric analysis and single-crystal X-ray diffraction.1 is a rare 2D→3D example with a 3-fold parallel interpenetration and polycatenaned architecture.2 features a scarce2D→2D example with a 3-fold parallel interpenetrating network which possesses polyrotaxane and polycatenane characters.Moreover,the luminescent properties of 1 and 2 have been discussed.

Synthesis, Structure and Luminescent Properties of Three 1D Chain Rare Earth Complexes

Three 1 D chain coordination polymers [Ln(pydc)2(H2 O)2]n·n Him(Ln = Dy(1), Gd(2), Sm(3), H2 pydc = pyridine-2,5-dicarboxylic acid, Im = imidazole), were solvothermally synthesized by the reaction of pyridine-2,5-dicarboxylic acid(H2 pydc), Ln(Ⅲ) salts and imidazole. They have been characterized by X-ray single-crystal diffraction, IR spectra, TGA analysis and elemental analysis. Structural analyses revealed that complexes 1~3 have similar 1 D chain structures and belong to P1 space group. It is noteworthy that complexes 1~3 exhibited excellent thermal stability and no weightlessness below 117 ℃. Meanwhile, 1 and 3 show characteristic fluorescence of corresponding lanthanide metal ions in solid state at room temperature.

Synthesis, Crystal Structure and Luminescent Property of the One-dimensional Chain Chlorodibenzyltin 2-Quininate

A one-dimensional chain chlorodibenzyltin 2-quininate has been synthesized and characterized by IR, NMR spectra and elemental analysis. The crystal structure has been determined by X-ray diffraction. The crystal belongs to the monoclinic system, space group I4（—） with a = 19.1171（10）, b = 19.1171（10）, c = 12.5158（6） , Z = 8, V = 4574.1（4） 3, Dc = 1.477 g·cm-3, μ（MoKα） = 1.252 mm-1, F（000） = 2032, R = 0.0259 and wR = 0.0723. In the complex, the tin atom is six-coordinated to adopt a distorted octahedral configuration with bridging carboxyl of quinoline-2-carboxylic acid. The result of fluorescence spectrum analysis shows that the title complex at room temperature exhibits an intense photoluminescence with maximum emission at 364.2 nm （λex = 303.0 nm）.

Synthesis, Crystal Structure and Luminescent Property of a Ag(Ⅰ) Coordination Polymer with a 3D Sandwich-like Framework

A new coordination polymer,{[Ag2（bpp）2（H2O）2]·bpdc·3H2O}n,derived from the ligand biphenyl-4,4＇-dicarboxylic acid（H2bpdc）,has been obtained through a hydrothermal technique（bpp = l,3-bis（4-pyridyl）propane）.Its single-crystal structure has been characterized by single-crystal X-ray diffraction,powder XRD,FT-IR,TGA and elemental analysis techniques.The single-crystal X-ray diffraction reveals that complex 1 consists of 1D infinite[Ag（bpp）（H2O）]n^（n＋）cationic chains,2D anionic layer constructed by bpdc anions and free water which provide charge compensation in the crystal structure.The 1D infinite[Ag（bpp）（H2O）]n^（n＋） cationic chains and 2D anionic layer are further stacked in-ABAB- fashion through intermolecular H-bonding to form a 3D sandwich-like framework.In addition,the luminescent property of complex 1 in the solid state at room temperature was investigated.

Synthesis, Crystal Structure and Catalytic Properties of a 2D Cobalt(II) Coordination Polymer Based on Mixed Ligands

A new Co（Ⅱ） metal-organic coordination polymer based on flexible bis（imidazole） and aromatic dicarboxylate co-ligands, namely [Co（bix）（nph）]n （H2nph = 3-nitrophthalic acid, bix = 1,4-bis（imidazole-l-ylmethyl）benzene）, has been hydrothermally synthesized and characterized by elemental analyses, TG, IR spectroscopy and single-crystal X-ray diffraction. It crystallizes in the triclinic space group Piwith a = 9.3767（14）, b = 10.1451（15）, c = 12.1488（17） A, α = 102.6450（10）, β = 108.856（2）, ）, = 98.807（2）°, V= 1035.3（3） A3, Z = 2, C22H17CoN5O6, Mr = 506.34, Dc = 1.624 g/cm^3, p = 0.882 mm^-1 and F（000） = 518. In the complex, the nph^2- ligands connect neighbouring cobalt atoms to form binuclear [Co（nph）]2 subunits, which are linked by pairs of bix ligands to form a 2D honeycomb-like （6,3） network. In addition, the compound is further extended into a 3D supramolecular architecture by π…π stacking interactions. Moreover, the luminescence and catalytic properties of the complex are investigated.

Synthesis, Crystal Structure and Properties of a New Cd(II) Complex Based on Mixed 5-Hydroxy-isophthalic Acid and 1-(1H-imidazol-4-yl)-3-(4H-tetrazol-5-yl)benzene Ligands

A new coordination polymer [Cd2（5-IPA）（HL）2（H20）2]＇4H20 （1） was prepared under hydrothermal conditions based on 5-hydroxy-isophthalic acid （5-H2IPA） with multi-N-donor ligand 1-（1H-imidazol-4-yl）-3-（4H-tetrazol-5-yl）benzene （H2L）. The complex was characterized by IR spectroscopy, TGA, X-ray powder and single-crystal diffraction. It crystallizes in the monoclinic system, space group C2/e with a = 23.6291（18）, b = 9.9847（8）, c = 17.7244（14） A, fl = 124.6180（10）°, V = 3441.4（5） A3, Z = 4, C28H30N12O11Cd2, Mr = 935.44, Dc = 1.805 g/cm^3,μ= 1.313 mm^-1, S = 1.055, F（000） = 1864, the final R = 0.049 and wR = 0.1315 for 2985 observed reflections （I 〉 2σ（I））. The central metal Cd（II） atoms with octahedral coordination geometry are six-coordinated by three oxygen and three nitrogen atoms. The HL- ligands from the deprotonated HzL connect Cd（II） atoms to form two-dimensional （2D） double-layer fes networks which are further pillared by 5-IPA2- ligands into a rare binodal （3, 4）-connected three-dimensional （3D） architecture with a （4·6·8）（4·62·83） fse-3,4-C2/c topology. Solid state luminescent property and sorption property of 1 have been investigated.

Synthesis, Crystal Structure and Luminescent Property of [Zn(C_(12)H_9O_3)_2(C_(10)H_8N_2)]_n·nH_2O

Under hydrothermal condition, the reaction of 2-naphthoxyacetic acid with ZnCl2 and 4,4′-bipyridine （4,4′-bipy） has afforded a new Zn（Ⅱ） compound, [Zn（C12H9O3）2（C10H8N2）]n·nH2O1, which was structurally characterized by single-crystal X-ray diffraction analysis. The crystal is of monoclinic, space group P21/c with a = 7.7335（2）, b = 19.3834（4）, c = 20.1707（4） A, β = 104.9830（10）°, V = 2920.82（11） A^3, C34H28ZnN2O7, Mr = 641.95, Z = 4, Dc = 1.460 g/cm^3,μ = 0.895 mm^-1, F（000） = 1328, R = 0.0406 and wR = 0.0876 for 4417 observed reflections （I〉 2σ（I）） Complex 1 consists of one-dimensional zigzag chains deriving from Zn（C12H9O3）2 units linked by 4,4′-bipy ligands, and lattice water molecules decorate between the chains. Non-covalent interactions, such as hydrogen-bonding and aromatic π-π interactions, lead to the formation of a 3D network structure. The thermogravimetric analysis （TGA） and luminescent property for 1 have also been studied in this paper.

Hydrothermal Synthesis, Crystal Structure and Fluorescence Properties of a Three-dimensional Triply-bridged Binuclear Zinc(Ⅱ) Complex [Zn_2(Mba)_3(Phen)_2EtOH)]·ClO_4

The novel complex [Zn2（Mba）3（Phen）2EtOH）]·ClO4 （Hrnba = methoxybenzoic acid, Phen = 1,10-phenanthroline, EtOH = ethanol） was synthesized by hydrothermal reactions, and its structure was determined by X-ray diffraction. The crystal belongs to the triclinic system, space group Pi with a = 1.15362（1）, b = 1.3655（3）, c = 1.61451（1） nm, α= 72.842（2）, β = 83.259（3）, y = 72.083（2）°, V = 2.3112（6） nm3, Z = 2,μ（MoKa） = 11.71 cm-1, F（000） = 1120, R = 0.0552 and wR = 0.1157 （I 〉 2σ（I））. The two centric zinc（H） ions in the complex locate in a distorted octahedral coordination geometry and a distorted trigonal bipyramid coordination geometry, respectively. Two bridging bidentate carboxyl groups and a μ2-O carboxyl group from three methoxybenzoic acids act as the bridge to link two Zn（Ⅱ） ions. The asymmetric units are connected by π-π packing interactions between aromatic rings to form a three-dimensional supramolecular network. The experimental results show a good fluorescence property for the complex.

Synthesis, Crystal Structure and Luminescence Property of a Cd(Ⅱ) Complex Assembled by 4-Carboxymethoxy Phenylacetic Acid

A new structure with the molecular formula [CdL]n was formed by CdSO4 with 4-carboxymethoxy phenylacetic acid （H2L） through the hydrothermal method. The complex was characterized by elemental analysis and infrared spectroscopy. The structure of the complex was determined by single-crystal X-ray diffraction, which is of monoclinic system, space group P21/c with a = 10.3887（2）, b = 7.10710（10）, c = 14.7212（2） , β = 120.6940（10）°, V = 934.65（3） 3, Dc = 2.278 g·cm-3, Z = 4, F（000） = 624, S = 1.022, the final R = 0.0187 and wR = 0.0487 for 2000 observer reflections （Ⅰ 〉 2σ（Ⅰ））. The center metal ion Cd（Ⅱ） in the complex is six-coordinated in a distorted octahedral geometry, and is connected with L ligands to form a 3D fishing net structure, which is a novel （3,6） network topology. The luminescence of the complex has been investigated, and the result reveals that it displays luminescent property in the voilet region.