Synthesis and Crystal Structure of a Two-dimensional Silver Framework Constructed by H_2idc (H_2idc = Iminodiacetic Acid)

A new compound formulated [Ag2(idc)](NO3)?H2O (H2idc = iminodiacetic acid) was synthesized under mild conditions and characterized by IR spectrum and single-crystal X-ray diffraction. The crystal crystallizes in the monoclinic system, space group of P21/n with a = 5.5029(2), b = 11.1316(5), c = 15.5319 (1) ?, β = 96.038(3)o, V = 946.15(6) ?3, Z = 4, R = 0.0619 and wR = 0.1606. Its structure is a 2D polymer, whose repeat units consist of dinuclear silver cluster coordinated by two bridging iminodiacetic acids. In the complex, the Ag(I) ions adopt three coordinate fashions, and the Ag-Ag metal-metal contacts of 2.8418 ? are observed.

Synthesis and Crystal Structure of a Heteronuclear Erbium and Yttrium Complex with Proline: [ErY(pro)_6(H_2O)_6] (ClO_4)_6

The title complex was synthesized in an aqueous solution at pH=3. 5,and its crystal structure was determined by X-ray diffraction methods. The com-plex is triclinic with space group P1, formula C30H66O42N6Cl6ErY, Mr,= 1651. 76, a=9. 860(2), b=13. 020(5), c= 13. 632(5) A ; a= 109. 32(3), β=110. 19(2), γ=100. 96(2)°, V= 1456(1 ) A3, Dc= 1. 884 g/cm3, Z= 1, F(000) =833, P= 2. 812mm-1 ;R=0. 046, wR(F2) =0. 123 for 4897 reflections with I>2(I). The complexis of an infinite chain structure with the neibouring metal ions connected by two bridging carboxyl groups from two different proline molecules. The erbium ion and the yttrium ion statistically lies at the position of the metal ion with M=1/2(Er+Y).

THE CRYSTAL STRUCTURE OF RARE EARTH COMPLEX WITH AMINO ACIDS Ⅱ The Crystal Structure of Gtutamate Comptex of Erbium Perchtorate

The crystat structure of {[Er;（L—Glu）;（H;O）;]（ClO;）;·3H;O);has been studied by X-ray diffraction. The crystal is monoctinic with space group P2;and cell parameters a=19.987（3） , b=16.505（3） , c=11.040（2） , β=104.69（1）;, V=3538（1） , Z=2, Dc=2.29 g. cm;, μ=53.2 cm;, F（000）=2384. The asymmetric unit contains two complex motecules and four centre ions. Each erbium （Ⅲ） is coordinated by five oxygen donors from four different glutamates and four oxygen donors from the aqua ligand to form a nine coordination potyhedron. The mean distances of Er—0 （carboxylate） and Er—Ow are 2.439 and 2.41 respectivety. The finat R and Rw are 0.043 and 0. 058, respectivety.

Investigation on Molecular and Crystal Structures of Metal Complexes with Aminopolycarboxylic Acids(Ⅰ)─Synthesis and Structure of Na_2[Fe~Ⅲ(ida)2]2·3H_2O

The crystal structure of the title complex salt has been determined by single-crystal X-ray structure analysis. The crystal data are as follows; Monoclinic, P21/c, a=15.6480(10)A,b=16.7870(10)A, c=10.347(2)A, β=90.790(10), V=2717.7(6)A3, Z=3, and R=0.0333 for 4789 unique reflections. The complex anion has a pseudo-octahedral structure distorted more than the CrⅢand CoⅢ analogs, in which cach iminodiacetato ligand (ida2-) is coordinated in a facial fashion with the two N atoms in a cis configuration, resulting in an unsyin-fac structure.

Synthesis and Crystal Structure of a New Copper(II) Complex with 4-Cyanobenzoic Acid

A new Cu（Ⅱ） complex [Cu（4-cba）（1,10-phen）（H2O）2]（NO3） （4-Hcba = 4-cyanobenzoic acid） has been synthesized by solvothermal reaction in an ethanol/water mixed solution at 100 ℃ and structurally characterized by single-crystal X-ray diffraction. Crystallographic data： C20H16CuN4O7, Mr= 487.91, triclinic, space group PI, a = 7.8420（2）, b = 9.1070（2）, c = 15.1140（6） A, a = 76.889（9）, β = 81.332（11）, γ = 74.844（ 11）°, V = 1009.89（5） A^3, Z = 2, Dc = 1.605 g/cm^3, F（000） = 498, μ = 1.134 mm^-1, the final R = 0.0379 and wR = 0.0865 for 2977 observed reflections with 1 〉 2σ（Ⅰ）. The Cu（Ⅱ） atom is coordinated by two terminal water molecules, one chelating 1,10-phen molecule and one monodentate 4-cba ligand to form a slightly distorted square pyramid. The title complex molecules are connected through hydrogen bonds and π-π stacking interactions to generate a 2D layered network. The thermogravimetric analysis of the title complex has also been discussed.

Hydrothermal Syntheses and Crystal Structures of Six Complexes Constructed from 1,3,5-Benzenetricarboxylic Acid and 4'-(4-Pyridyl)-2,2':6',2''-terpyridine Mixed Ligands

Six new transition metal complexes, [Zn（HBTC）（PYTPY）]n·n PYTPY（1）, [Cu（HBTC）（PYTPY）]n·n PYTPY（2）, [Co（HBTC）（PYTPY）]n·n DMF（3）, [Mn（HBTC）（PYTPY）]n·n DMF（4）, [Cd（HBTC）（PYTPY）（H2O）]n·2nH2O（5）, and [Co（HBTC）（PYTPY）（H2O）2]（6）,（H3BTC = 1,3,5-benzenetricarboxylic acid, PYTPY = 4＇-（4-pyridyl）-2,2＇：6＇,2＇＇-terpyridine, DMF = N,N？-dimethylformamide）, have been synthesized and characterized by elemental analysis, IR and X-ray single-crystal diffraction. Complexes 1~5 all feature one-dimensional chain structures, and complex 6 exhibits a zero-dimensional structure. Complexes 1~5 present three-dimensional（3D） supramolecular frameworks via π-π stacking interactions, whenas 6 has also a 3D supramolecular structure assembled by hydrogen bonding. Meanwhile, complexes 1 ~ 6 exhibit the thermal stabilities and photoluminescent properties.

Hydrothermal Synthesis and Crystal Structure of a New One-dimensional Nickel(Ⅱ) Complex with 2-Pyridinecarboxyic Acid and 4,4′-Bipyridine Ligands

A new metal-organic coordination polymer [Ni[（2-pya）2（4,4′-bipy）]n·6nH2O （2-pya = 2-pyridinecarboxylic acid, 4,4′-bipy = 4,4′-pyridine） 1 has been hydrothermally synthesized and structurally characterized by elemental analysis, IR spectrum, TG and single-crystal X-ray diffraction. The complex crystallizes in tetragonal, space group I4 1/α with a = b = 22.5642（19）, c = 10.7118（18） A, V = 5453.8（11） A^3, C22H28N4NiO10, Mr= 567.19, Dc = 1.382 g/cm^3, μ（MoKα） = 0.769 mm^-1, F（000） =2368, Z = 8, the final R = 0.0572 and wR = 0.1254 for 1401 observed reflections （I 〉 2σ（I））. It exhibits a one-dimensional chain-like structure by mixed ligands of 2-pyridinedicarboxylic acid and 4,4′-pyridine.

Syntheses and Crystal Structures of Three Ag(Ⅰ) Complexes with Chloro-phenylacetic Acid and Nitrogen Heterocyclic Ligand

Three new coordination polymers {[Ag2（2,4-DCPA）（4,4＂-bipy）2（NO3）].（H20）}, （1）, [Ag（2,4-DCPA）（bpp）], （2） and {[Ag（4-DCPA）（bpp）]＇（H20）}, （3）, were synthesized by evaporation methods using 2,4-dichlorophenylacetic acid （2,4-DCPA）, 4-chlorophenylacetic acid （4-DCPA）, 4,4＂-dipyridyl （4,4＂-bipy）, 1,3-bis（4-pyridyl）propane（bpp） and AgNO3. Compound 1 crystallizes in monoclinic, space group P21/c with a = 10.035（2）, b = 17.796（3）, c = 16.448（2） A, fl = 104.086（2）°, V= 2705.9（2） A3, Dc = 1.893 g/cm-3, C28H23C12NsO6Ag2, Mr = 812.15, F（000） = 1608,μ（MoKot） = 1.615 mm-1, Z = 4, R = 0.0310, wR = 0.0832 for 4357 observed reflections （I 〉 20（/））, and R = 0.0362, wR = 0.0873 for all data. Compound 2 crystallizes in monoclinic, space group P21/c with a = 9.840（2）, b = 24.971（5）, c = 9.3301（2）°, fl = 117.504（2）°, V= 2033.5（7） A3, Dc = 1.666 g/cm3, C2tH19C12N202Ag, Mr = 510.15, F（000） = 1024,/I（MoKa） = 1.273 mml, Z= 4, R = 0.0315 and wR = 0.0680 for 2853 observed reflections （1 〉 20（/）） and R = 0.0454, wR = 0.0736 for all data. Compound 3 crystallizes in monoclinic, space group P21/n with a = 15.472（4）, b = 9.000（2）, c = 16.262（4） A, fl = 112.049（4）°, V = 2099.0（8） A3, Dc = 1.562 g/cm-3, C2H22C1N203Ag, Mr = 493.73, F（000） = 1000, μ（MoKa） = 1.111 mm-1, Z = 4, R = 0.0296, wR = 0.0821 for 3059 observed reflections （I 〉 2δ-（I））, and R = 0.0398, wR = 0.0986 for all data. The complexes were characterized by elemental analysis, FT-IR, thermogravimetrie analysis （TGA） and X-ray single-crystal structure analysis. Fluorescence properties of complex 3 and PXRD of 1 and 2 have been studied. As a result, in complex 1, the Ag（I） ion is surrounded by two nitrogen atoms from two bipy ligands to form an infinite chain, and adjacent Ag-bipy chains produce ＂＇rungs＂ of a ladder by silver ions contact. And in complexes 2 and 3, the two-dimensional ,β-sheet like layers are obtained by Ag……Ag interactions.

Synthesis, Crystal Structure and Thermal Stability of a New Binuclear Cu(Ⅱ) Complex with 2-Benzoylbenzoic Acid as the Ligand

A new complex Cu2（o-C6H5COC6H5COO）4（C10H8N2）2（H2O）2 with 2-benzoylben- zoic acid and 2,2′-bipyridine as ligands has been synthesized in mixed methanol and water solvent. Crystal data are as follows： monoclinic, space group Co, a = 14.0133（14）, b = 16.0409（16）, c = 30.372（3） A, β = 100.8950（10）°, V = 6704.1（12） A3, Dc = 1.364 g/cm3, Z = 8,μ（MoKa） = 0.704 mml, F（000） = 2840, the final R= 0.0552 and wR = 0.1431. In the crystal structure, the whole molecule consists of two copper ions, four 2-benzoylbenzoic acid molecules, two 2,2′-bipyridine molecules and two water molecules. Each central copper ion is coordinated with two nitrogen atoms from one 2,2′-bipyridine molecule and three oxygen atoms from two 2-benzoylbenzoic acids and one water molecule, respectively, giving a distorted tetragonal pyramidal geometry. Thermal stability properties of the complex were investigated.

Hydrothermal Synthesis and Crystal Structure of a New One-dimensional Cobalt(Ⅱ) Complex with 2-Pyridinecarboxyic Acid and 4,4′-Bipyridine Ligands

A new metal-organic coordination polymer [Co（2-pya）2（4,4＇-bipy）]2n-[（4,4＇- bipy）0.5· H2O]2n （2-pya = 2-pyridinecarboxylic acid, 4,4＇-bipy = 4,4＇-bipyridine） 1 has been hydrothermally synthesized and structurally characterized by elemental analysis, IR spectrum, TG and single-crystal X-ray diffraction. The complex crystallizes in tetragonal, space group I41/a with a = b = 22.719（2）, c = 10.710（2）/k, V = 5527.8（14） A3, C54H46N10Co2O10, Mr= 1112.87, Dc = 1.337 g/cm3,μ（MoKa） = 0.665 mm-1, F（000） = 2296, Z = 4, the final R = 0.0633 and wR = 0.1096 for 1261 observed reflections （I 〉 2σ（I））. It exhibits a one-dimensional chain-like structure constructed by mixed ligands of 2-pyridinedicarboxylic acid and 4,4＇-bipyridine.

Synthesis and Crystal Structure of a New cis-Dioxovanadium (V) Complex with Pyruvic Acid Isonicotinyl Hydrazone (PAINH)

A new cis-dioxovanadium （V） complex [VO2（C9H8N3O3）]（C5H5N） involving a carboxyl group coordination employing a tridentate Schiff Base derived from pyruvic acid and isonicotinyl hydrazide is reported. This complex crystallizes in triclinic, space group P1^- with a = 7.3522 （12）, b = 7.8376（13）, c = 14.898（2） ,A°, a = 84.010（2）, β = 86.568（2）, γ= 64.586（2）°, V = 771.1（2）A °^3 ,Z = 2, F（000） = 376, Mr = 368.22, D, = 1.586 g/cm^3, g = 0.677 mm ^-1, R = 0.0421 and wR = 0.1253. The vanadium atom of the dioxovanadium （V） is five-coordinated to furnish a distorted trigonal bipyramid geometry.

Synthesis, Crystal Structure, Luminescent Property and DNA-Binding of a Cadmium Complex with 2,4-Bis-oxyacetate-benzoic Acid

A complex [Cd2Na2（BOABA）2（H2O）8]·H2O（1） was synthesized by using 2,4-bisoxyacetate-benzoic acid（H3BOABA） and Cd（OH）2. It was characterized by elemental analysis, IR spectra, and single-crystal X-ray diffraction. Complex 1 shows a two-dimensional 3-connected rigid plane. The interactions between the ligand and its complex with DNA were studied by Et Br fluorescence probe. Photoluminescent studies indicate that the complex may be excellent candidates for potential photoactive materials.

Synthesis and Crystal Structure of a Novel Ternary Ni(II) Complex with 2-Hydroxyl-1,10- phenanthroline and 2-Hydroxynicotinic Acid as Ligands

A novel ternary complex of [NiL1L2·2H2O]·NO3·H2O （L1 = 2-hydroxyl-1,10-phenanthroline （HOphen）, L2 = 2-hydroxynicotinic acid （H2nicO）） was synthesized, and its crystal structure was determined by X-ray diffraction and further characterized by infrared and elementary analysis. The title complex （C18H18NiN4O10, Mr = 509.07） belongs to the triclinic system, space group P1^- with a = 712490（7）, b = 11.0164（10）, c = 13.3864（13）A, α = 91.6040（10）,β= 98.8620（10）, γ= 107.1140（10）°, V= 1006.43（17）A^3, Z = 2, Dc = 1.680 g/cm^3,μ= 1.032 mm^-1, F（000） = 524, the final R = 0.0461 and wR= 0.1238. In the complex, the Ni（H） ion is six-coordinated to assume a distorted octahedral geometry, and a 3D supramolecular network comes into being via weak intermolecular interactions of X-O--.H （X = N, O）.

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.

Synthesis, Crystal Structure and Properties of a Europium Complex with 3-Iodobenzoic Acid and 2,2'-Bipyridine

The complex [Eu（3-IBA）3·2,2＇-bipy]2 was synthesized from 3-iodobenzoic acid （3-HIBA）, 2,2＇-bipyridine （2,2‘-bipy） and EuCl3·6H2O by hydrothermal synthesis, and its crystal structure was determined by X-ray single-crystal diffraction. It is of triclinic, space group Pi, with a = 10.958（2）, b = 12.311（3）, c = 12.556（3） A, α = 81.549（3）, β = 82.404（4）, γ = 78.348（3）°, Mr = 1049.15, V= 1631.7（6） A3, Z = 1, Dc = 2.135 g/cm^3, F（000） = 980, 2（MoKa） = 0.71073 A,μ（MoKa） = 4.804 mm^-1, the final R = 0.0329 and wR = 0.0723 for 4640 observed reflections with I 〉 2σ（I）. The Eu（Ⅲ） ion is eight-coordinated and two Eu（Ⅲ） ions are held together by four 3-iodobenzoate groups in the bidentate bridging mode. The complex was characterized by DTA-TG, IR, UV and fluorescence spectra.

Syntheses and Crystal Structures of Two Diethyltin Complexes of N-Salicylidene-α-amino Acid

Two novel diethyltin（IV） complexes of N-salicylidenevaline （H2L1） and N-Sali- cylidenetryptophan （H2L^2）, Et2SrtL^1 1 and Et2SnL^2 2, were synthesized and characterized by elemental analysis, IR, ^1H NMR and X-ray single-crystal diffraction analysis. Complex 1 belongs to the trigonal system, space group R-3 with a = b = 19.2730（5）, c = 23.6890（13）A^°, V= 7620.4（5） A^°^3, Z = 6, Dc= 1.553 g/cm^3,μ= 1.518 mm^-1, F（000） = 3600, R = 0.0238 and wR = 0.0636. Complex 2 is of monoelinie system, space group P21/c with a = 13.7550（8）, b = 11.5425（7）, c = 12.7876（7）A^°, β= 93.585（1）°, V = 2026.3（2） A^°^3, Z = 4, Dc= 1.548 g/cm^3,μ = 1.286 mm^-1, F（000） = 976, R = 0.0298 and wR = 0.0722. Complex 1 is a cyclic trimer with a macrocyclic 12-membered ring structure formed by the bidentate bridging coordination of carboxylate group to tin atoms. The tin atom is six-coordinated in a distorted octahedral geometry. In complex 2, the distorted trigonal bipyramidal Et2SnL2 units are linked into polymeric chains by the weak Sn…O interaction involving Sn and the earbonyl O of an adjacent ligand, and the chains are further connected by intermolecular N-H…O hydrogen bonds to form a two-dimensional supramolecular structure.

Synthesis and Crystal Structure of a Lanthanum(Ⅲ) Complex with Chelidamic Acid

A new lanthanum complex, （H3O）2[La（C7H3NO5）2（H2O）212.3（H2O） or （HaO）E[La（HChel）2（HEO）E]2.3（H2O） 1 （H3Chel = 4-hydroxypyridine-2,6-dicarboxylic（chelidamic） acid）, has been prepared by the hydrothermal reaction, and its crystal structure was determined based on single-crystal diffraction data. Compound I crystallizes in triclinic, space group Pi with a = 9.6939（19）, b = 10.176（2）, c = 11.502（2）A, α = 111.52（3）, β = 93.74（3）, γ = 103.33（3）°, V = 1013.0（3）A3, Dc = 1.912 g/cm3, Z = 1, Mr = 1166.40, p = 2.188 mm-1, 2（MoKa） = 0.71073 A and F（000） = 574. The final R = 0.0342 and wR = 0.0737 for 4080 observed reflections with I 〉 2σ（I）, and R = 0.0429 and wR = 0.0772 for all data. Compound 1 contains two lanthanum ions, four chelidamic acid ligands, four coordinated water molecules, two hydroniums, and three discrete water molecules. The LaⅢ atom is ten-coordinated by four oxygen and two nitrogen atoms from two tridentate chelating chelidamic acid ligands, two carboxylic oxygen atoms from an adjacent chelidamic acid ligand and two coordinated water molecules, leading to a distorted dodecahedral geometry. A three-dimensional network is formed by H-bonds.

Synthesis and Crystal Structure of Palladium(Ⅱ) Complex with 2,2’-Bipyridine-3,3’-dicarboxylic Acid

The title complex Pd（H2BDA）Cl2·2DMSO （C16H14Cl2N2O6PdS2, H2BDA = 2,2＇- bipyridine-3,3＇-dicarboxylic acid） has been synthesized and characterized by IR spectra, elemental analysis and ^1H NMR spectra. Its structure was determined by single-crystal X-ray diffraction analysis. The complex crystallizes in the monoclinic system, space group P2（1/c） with a = 1.3604（6）, b = 1.2606（6）, c = 1.3521 （6） nm, β = 103.677（7）°, V = 2.2530（17） nm^3, Mr = 571.75, Z = 4, Dc = 1.686 g/cm^3,μ = 1.280 mm^-1, F（000） = 1136, R= 0.0405 and wR= 0.0908. The complex presents a planar quadrangle arrangement and is assembled via hydrogen bonds.

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.