Hydrothermal Synthesis and Crystal Structure of [Cu(en)2(H2O)]2{PW11.5Cu0.5O40[Cu(en)2]}·2H2O

A transition metal substituted polyoxotungstate,[Cu(en)2(H2O)]2{PW11.5Cu0.5O40 [Cu(en)2]}·2H2O1 based on Keggin frameworks ,has been hydrothermally synthesized and charac-terized by IR,TGA and single-crystal X-ray structural analysis.It is interesting to find that the structure unit contains two different valence cations,namely,one[Cu(1)(en)2(H2O)] and one [Cu(2)(en)2(H2O)]2 .Data for the crystal:orthorhombic system,space group Pbca,a=21.585(2),b=20.695(2),c=26.137(3)(A),V=11675(2)(A)3,Z=8,Mr=3428.23,Dc=3.901 g/cm3,F(000)=12156,μ(MoKα)=23.932mm-1,the final R=0.0468 and wR=0.0969 for 6927 observed reflections(Ⅰ＞2σ(Ⅰ)).     

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.     

Synthesis and Crystal Structure of （H3O）2[Cu3Cl3（H2O）3（NC9H12.5O6）2]

1 INTRODUCTION The polydentate ligand nitrilotripropionic acid, H3ntp[N(CH2CH2COOH)3], has attracted conside- rable research interest in constructing coordination polymers, designing organic-inorganic hybrid mate- rials[1], synthesizing supramolecular compounds[2], etc. due to its high degree of flexibility with three carboxylic acid moieties allowing for a variety of coordination through oxygen atoms[3]. It also pro- vides other versatile properties such as the possibili- ty of inter-…     

Hydrothermal Synthesis and Crystal Structure of a Polyoxometalate- based Complex [Cu^I（phen）2]4（SiW12O40）

A new hybrid polyoxometalate-based complex, [Cu^I（phen）214（SiW12O40） （phen = 1,10-phenanthroline）, has been synthesized by hydrothermal method and characterized with the aid of elemental analysis, IR, UV spectra and thermal analysis studies. The result of X-ray crystallography analysis exhibits that the title compound crystallizes in the orthorhombic space group P212121, and the formula is C96H64N16Cu4SiW12O40. Crystal data： a = 18.3574（14）, b = 21.1952（16）, c = 27.992（2）A, Mr = 4570.08, V = 10891.4（14）A^3, Z = 4, Dc = 2.787 g/cm^3,μ = 13.478 mm^-1, R = 0.0364, wR = 0.0638 （I 〉 2σ（I）） and F（000） = 8360. The complex consists of one α-Keggin anion [SIW12O40]^4- and four discrete [Cu^I（phen）2]^＋ cations. The valence sum calculations for the Cu atoms suggest that all four Cu atoms are in the ＋1 oxidation state.     

Hydrothermal Synthesis and Crystal Structure of a New Polyoxovanadate： [Mn（en）3]2en0.5[HV8VV8IVO38（CI）]·4.5H2O （en = Ethylenediamine）

A new compound has been synthesized under hydrothermal conditions and characterized by IR, elemental analysis, XPS and single-crystal X-ray diffraction analysis. The title compound [Mn（en）3]2en0.5[HV8VV8IVO38（CI）]·4.5H2O crystallizes in monoclinic, space group C2/c, with a = 17.016（4）, b = 18.858（4）, c = 18.872（4） A, β = 93.667（4）°, V = 6043（2）A3, Z = 4, Dc = 2.242 g/cm3, Mr = 2040.12, F（000） = 4020,μ = 2.895 mm-1, Rint = 0.0921, R = 0.0649 and wR = 0.1325. Single-crystal X-ray structure analysis indicates that the title compound consists of a polyanion [HV8VV8IVO38（CI）]4- cage, two [Mn（en）3]2^2＋ cations, four and a half lattice waters and a half ethylenediamine. In addition, intermolecular O-H...N, O-H...O, N-H...O and C-H...O hydrogen bonds link the molecules together to form a three-dimensional structure.     

Synthesis and Crystal Structure of the Copper Complex {[Cu（CH3COO）2（bbtz）]（H2O）2}n

1 INTRODUCTION The design and synthesis of metal-organic frame- work structures have been extensively studied due to their unexpected properties for potential applications as functional materials as well as the intriguing ar- chitectures and topologies[1～4]. When rigid bifunc- tional ligands are used to connect metal centers, to- pology of the network is usually determined by the coordination geometry of the central metal prefer- ence. Contrary to rigid ligands, the bifunctional fle- xib…     

Synthesis and Crystal Structure of Cu2（pba）（bpy）2Cl2.4H2O

1　ＩＮＴＲＯＤＵＣＴＩＯＮＴｈｅｃｏｏｒｄｉｎａｔｉｏｎｃｈｅｍｉｓｔｒｙｏｆｍｕｌｔｉ ｓｕｂｓｔｉｔｕｔｅｄｏｘａｍｉｄｅｓｉｓｏｆｉｍｐｏｒｔａｎｃｅｔｏａｗｉｄｅｖａｒｉｅｔｙｏｆｃｈｅｍｉｃａｌ[1 ] ,ｂｉｏｌｏｇｉｃａｌ[1 ] ａｎｄａｐｐｌｉｅｄｓｙｓｔｅｍｓ[2 ,3] .Ｔｈｅｍａｇｎｅｔｉｃ[4,5]ａｎｄｓｐｅｃｔｒｏｓｃｏｐｉｃ[6 ,7] ｐｒｏｐｅｒｔｉｅｓｏｆｔｈｅｏｘａｍｉｄｅｃｏｍｐｌｅｘｅｓａｒｅｖｅｒｙｉｎｔｅｒｅｓｔｉｎｇ .Ａｌｏｔｏｆｍｏｎｏｎｕｃｌｅａｒａｎｄｂｉｍｅｔａｌｌ…     

Synthesis, Character and Crystal Structure of the Complex {Er（DMSO）7} PW12O40

The synthesis, X-ray crystal structure, thermal properties and electrochemistry of the new complex formulated as {Er(DMSO)7}PW12O40 are reported. The single-crystal X-ray analysis reveals that the crystal crystallizes in the monoclinic system, space group P21/c with a = 11.767(2), b = 14.909(3), c = 34.905(7) , β = 98.97(3)°, Mr = 3591.33, V = 6049(2) 3, Dc = 3.944 g/cm3, Z = 4, GOOF = 1.098, F(000) = 6340, R = 0.0490 and wR = 0.1202. Crystal structure analysis indicates that the Er(Ⅲ) is seven-coordinate with a distorted pentagonal bipyramid and combines to the anion [PW12O40]3- via static electric force.     

Synthesis and Crystal Structure of the Polymorphic Isomer [Cu（dafone）2（H2O）2]（Hphth）2

1 INTRODUCTION The metal-containing supramolecular frame- works can be constructed through coordinate cova- lent or supramolecular contacts such as hydrogen- bond and π-π stacking[1 ～ 3]. Extended networks possessing higher dimensionalities can be obtained by assembly of coordination polymers (or comple- xes) with lower dimensionalities via hydrogen bond interactions[4～13]. However, normally the higher di- mensional networks are generated by one-dimen- sional chains through hydrogenbo…     

Hydrothermal Synthesis and Crystal Structure of a Keggin Polyoxometalate [Co^Ⅱ（2,2′-bipy）2（H2O）]2[SiW^Ⅵ12O40]·2H2O

A Keggin-type tungstosilicate compound [Co^Ⅱ（2,2′-bipy）2（H2O）]2[SiW^Ⅵ12O40]·2H2O 1 （bipy = bipyridine） was prepared by a hydrothermal method for the first time. Single-crystal X-ray diffraction revealed that 1 （C40H40Co2N8O44SiW12） crystallizes in the triclinic system, space group P1 with a = 10.4979（6）, b = 13.3946（7）, c = 13.5756（8）A, α= 70.0769（18）, β = 68.910（3）, γ = 74.186（4）°, V = 1649.84（16）A^3, Mr = 3688.95, Z = 1, Dc = 3.713 mg·m^-3, μ = 21.432 mm^-1, F（000） = 1644, S = 1.058, the final R = 0.0511 and wR =0.1023 for 6523 observed reflections （I 〉 2σ（I））. Compound 1 consists of two coordinated cation fragments [Co^Ⅱ（2,2′-bipy）2（H2O）]^2＋, one normal Keggin polyanion unit [SiW^Ⅵ12O40]^4- and two lattice water molecules. To be noted, each polyanion unit is linked to two cation fragments by its two surface terminal oxygen atoms and two cobalt atoms of two cation fragments forming an organic-inorganic hybrid unit in 1. Furthermore, the compound shows strong photoluminescence property in the solid state at room temperature.     

Synthesis and Crystal Structure of [Cu2（DMF）（H2O）（C7H4NO4）2（C7H3NO4）]2·3.5DMF

A new copper（H） complex [Cu2（DMF）（H2O）（C7H4NO4）2（C7H3NO4）]2-3.5DMF has been synthesized and its structure was determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P1^- with a = 10.722（3）, b = 18.170（4）, c = 20.923（7）A,α = 105.297（9）, β = 101.701（10）, γ = 105.74（1）°, V= 3615（1）A^3, Z = 2, C58.50H64.50Cu4N1l.50O3150, Mr = 1686.90, Dc = 1.550 g/cm^3,μ= 1.255 mm^-1, F（000） = 1728.00, T = 150（2） K, the final R = 0.0640 and wR = 0.173 for 11310 observed reflections with I 〉 2σ（I）. In the crystal, each formular unit consists of two dinuclear copper（H） compounds, between which the O-H…O hydrogen bonds exist. Each Cu^Ⅱ cation is six-coordinated in an octahedral geometry. The intermolecular hydrogenbonding interaction leads to a 3-D framework of the title compound.     

Hydrothermal Synthesis, Crystal Structure and Electrochemical Properties of Complex Zn（phen）（m-CBA）2（H2O）

A novel complex Zn(phen)(m-CBA)2(H2O) with m-chlorobenzoic acid (m-CBA), 1,10-phenanthroline (phen) and zinc chloride has been hydrothermally synthesized and characterized. Crystal data for this complex: triclinic, space group P1, a = 0.8361(5), b = 1.2455(7), c = 1.3107(7) nm, α = 115.637(8), β = 91.014(9), γ = 104.857(8)o, V = 1.1763(11) nm3, Dc = 1.623 g/cm3, Z = 2, F(000) = 584, GOOF = 1.078, the final R = 0.0453 and wR = 0.1192. Structure analysis shows that the zinc ion coordinates with two nitrogen atoms of one 1,10-phenanthroline molecule, three oxygen atoms from two m-chlorobenzoic acid molecules and one water molecule, giving a distorted square-pyramidal coordination geometry. The cyclic voltametric behavior of the complex was also investigated.     

Synthesis and Crystal Structure of [Mn（DPMT）2Cl2（H2O）2]

The title compound [Mn(DPMT)2Cl2(H2O)2] (DPMT = 1-[[2-(2,4-dichlorophenyl)- 1,3-dioxolan-2-yl]methyl]-1H-1,2,4-triazole) was synthesized by the reaction of MnCl2·4H2O and DPMT in ethanol solution and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c with a = 23.913(4), b = 7.8883(13), c = 8.6291(14) , β = 95.816(3)o, V = 1619.4(5) 3, Z = 2, C24H26Cl6MnN6O6, Mr = 762.15, Dc = 1.563 g/cm3, μ = 0.950 mm-1, S = 1.045, F(000) = 774, R = 0.0462 and wR = 0.0981. The molecular structure is a centrosymmetric conformation, and two ligands are symmetrically located on both sides of the Mn atom. The manganese atom is surrounded by two nitrogen atoms from ligands, two chlorine atoms and two oxygen atoms from water molecules to form a slightly distorted octahedral geometry.     

Synthesis and Crystal Structure of [La（BTC）（H2O）6]n

1 INTRODUCTION desired topologies owing to their rich coordination modes[8~12] and we have been exploring the chemi- The assembly of metal-organic infinite frame- stry of coordination polymers constructed by tran- works via coordination of metal ions with multifunc- sition metals and benzoic multicarboxylic acids[13~16]. tional organic ligands is a field of increasing inte- In addition, lanthanide ions have high affinity for rest[1~4]. A rational designed and predictable coor- hard donor a…     

Synthesis and Crystal Structure of a Cu^2＋ Supramolecular Complex [Na2Cu（BTA）2（H2O）8]·H2O with a Three-dimensional Network Structure

A three-dimensional Cu^2＋ supramolecular complex [Na2Cu（BTA）2（H2O）8]·H2O 1 （H2BTA = bistetrazolylamine） was synthesized by reacting the aqueous solution of CuSO4·5H2O and H2BTA under stirring. The crystal structure of 1 was determined by single-crystal X-ray diffraction. The result indicates that 1 crystallizes in triclinic, space group P1, with a = 7.0518（2）, b = 12.2692（2）, c = 13.8583（3） A, α = 115.7260（10）,β = 93.2440（10）, γ = 98.3610（10）°, Mr = 573.90, V= 1059.01（4） A^3, Z = 2, De= 1.800 g·cm^-3,μ（MoKα） = 1.155 mm^-l, F（000） = 586.0, S = 1.074, the final R = 0.0273 and wR = 0.0744 for 4334 observed reflections with I 〉 2σ（I）. The Cu^2＋ ion is five-coordinated with a N4O1 donor set with r = 0.153 according to the method of Addison et al. And the Na^＋ ions form an infinite main chain through bridging O atoms from coordinated water molecules. In 1, a three-dimensional supratnolecular network is formed by O-H….O, O-H…N, N-H…O and N-H…N hydrogen bonds.     

Hydrothermal Synthesis and Crystal Structure of a Novel Composite Keggin-type Arsenotungstate： [Ni（phen）2] [Hphen] （AsW12O40）

A novel polyoxometalate-based composite compound [Ni(phen)2][Hphen](AsW12O40) (phen = 1,10-phenanthroline) 1 has been hydrothermally synthesized and characterized by elemental analysis, IR, TGA, ESR spectroscopy and single-crystal X-ray diffraction. Each structure unit of 1 consists of one polyoxoanion AsW12O403-, one free phenanthroline molecule and one coordination cation [Ni(phen)2]2+. The title compound crystallizes in the orthorhombic system, space group P212121, with a = 12.2383(7), b = 21.0884(11), c = 22.3237(12) , V = 5761.4(5) 3, Mr = 3520.44, Z = 4, Dc = 4.059 g/cm3, F(000) = 6204, μ(MoKα) = 24.844 mm-1, GOF = 1.022, the final R = 0.0376 and wR = 0.0742 (I > 2σ(I)) for 865 parameters and 9637 observed reflections with I > 2σ(I).     

Synthesis,Crystal Structure and Electrochemical Properties of a One-dimensional Chain Coordination Polymer [Cu（phen）（2,4,6-TMBA）2（H2O）]n

A one-dimensional chain coordination polymer [Cu（phen）（2,4,6-TMBA）2（H2O）]n has been synthesized by reacting 2,4,6-trimethyl-benzoic acid, 1,10-phenanthroline and Cu（Ⅱ） perchlorate and its structure was characterized. Crystal data for this complex： tetragonal, space group I41, a = 2.0293（3）, b = 2.0293（3）, c = 1.3758（2） nm, α =β= γ = 90°, V= 5.6657（13） nm3, Dc= 1.379 g/cm3, Z = 8, μ（MoKa） = 0.815 mm-1, Mr = 588.14, F（000） = 2456, S = 1.047, R = 0.0459 and wR = 0.1053. The crystal structure shows that two neighboring Cu（Ⅱ） ions are linked together by one bridging-chelating 2,4,6-trimethyl-benzoic group, forming a one-dimensional chain structure. Each Cu（Ⅱ） ion is coordinated with two nitrogen atoms from one 1,10-phenanthroline molecule, three oxygen atoms from three 2,4,6-trimethyl-benzoic acid molecules and one oxygen atom from one water molecule, giving a six-coordinate distorted octahedral coordination geometry. The cyclic voltammetry behavior of the complex was also investigated.