Synthesis and Crystal Structure of the Polyoxometalatebased Complex [Mn（DMSO）5H2O]2SiMo12O40

1 INTRODUCTION The design and assembly of organic-inorganic solid-state materials with active physical properties, such as materials with electrical, magnetic and opti- cal properties, has become a focus of a great deal of interest in recent years[1, 2].…     

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.     

Solvothermal Synthesis and Crystal Structure of a Novel Inorganic—Organic Hybrid Material,Fe2O（OH）（C5H4NCOO）SO4

IntroductionThereisatremendousactivityforthepastyearsintheareaofinorganic organichybridmaterialsinviewoftheirdi versifiedstructuresandinterestingproperties.1,2 Theeffortshavebeenmadeinsynthesizingandcharacterizingtheclassofmaterials.3Thecontrolofinorganicstructurebyanorganiccomponentrevealsaninteractivestructuralrelationinthema terials .4 Assemblyofaninorganic organichybridmaterialcanbeachievedbyselectingorganiccomponents (multidentateligands)andinorganiccomponents (transitionmetalions ,metalo…     

Synthesis and Characterizaion of a New Inorganic-organic Sulfate Compound ——Crystal Structure of [Ni （H2O）6][H2N （C2H4）2NH2]（SO4）2

IntroductionResearchactivitiesintheareaofchemicaldiversi tyofinorganiccompoundstemplatedbyorganicamineshavebeengrowingenormouslyduringthepastfew years[1] .Mostofthosecompoundsarebasedonoxygen containingmaterialsconsistingofelementsfromthemainblockoftheperiodictableandthetran sitionmetals.Thosematerialsareofgreatinteresttobothindustrialandacademicfieldsduetotheircatalytic ,adsorbtionandion exchange proper ties[2— 4 ] .Recently ,acommonlyusedmethodofhy drothermalsynthesishasinvolvedtheincorpora…     

Synthesis,Electrocatalytic Properties and Crystal Structure of a New Organic—Inorganic Hybrid Constructed from Dodecamolybdophosphoric Acid and Benzotriazole

IntroductionIn the last few years there has been a rapidlygrowing number of reports in the literature ad-dressing the use of polyoxometalate- based hybridmaterials as catalysts,non- linear optical materialsand anti- virus drugs[1— 5] . In all the cases men-tioned above,the size,the shape and the chargesof the inorganic counter anions strongly affect theproperties of the materials. Polyoxometalates arelarge in size and high in electron accepting abili-ty[6] .They can form novel compounds with …     

Synthesis and Crystal Structure of a New 2D Honeycomb—like Cadmium （Ⅱ） Complex with Tripodal Ligand

A new cadmium (II) coordination polymer, [Cd(TTTMB)₂]‐(SO₄) · 21H₂O, where TTTMB =1,3, 5‐tris (imidazol‐1‐yl‐methyl)‐2,4,6‐trimethylbenzene, was obtained by self‐assembly of tripodal ligand TTTMB with CdSO₄·2.7H₂O in acetonitrile, and characterized by X‐ray crystallography. The crystal data belongs to monoclinic space group C_c with cell parameters a = 1.16891(4) nm, b=2.06671(6) nm, c = 2.48185(7) nm, β = 97.8560(10)°, R = 0.0487, wR = 0.1211. The results of structure analysis indicate that each TTTMB ligand coordinates three metal atoms and in turn each Cd(II) atom with octahedral coordination geometry connects six nitrogen atoms of imidazole group from six different TTTMB ligands to produce a 2D honeycomb network structure. There are a lot of water molecules linked by hydrogen bonds and occupied the channels formed intra‐ and inter‐sheets.     

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).     

A Novel Complex of Na（I）-Nitronyl Nitroxide [Na（NIT- 1＇-MeBzIm）3]ClO4： Synthesis and Crystal Structure

A novel complex [Na（NIT-1＇-MeBzIm）3]ClO4 （NIT-1＇-MeBzIm = 2-{2＇-[（1＇- methyl）benzimidazolyl]}-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide） has been prepared and structurally characterized by elemental analysis, IR spectra and X-ray diffraction methods. The title complex crystallizes in trigonal, space group P3 and Z = 2. Crystal data： C45H57ClN12NaO10, Mr = 984.47, a = 13.9411（8）, b = 13.9411（8）, c = 14.8622（16） A, γ= 120°, V= 2501.5（3） A^3, Dc = 1.307 g/cm^3, μ（MoKα） = 0.152 mm^-1, F（000） = 1038, R = 0.0637 and wR = 0.1813 for 1957 observed reflections with I 〉 2σ（I）. X-ray analysis reveals that the Na（I） ion is six-coordinated with three NIT-1＇-MeBzlm radicals. As we know, three radicals coordinating to the Na（I） ion in the main group by a chelate way is the first example. The Na（I） ion resides in a distorted octahedron with a facial configuration. Meanwhile, the intermolecular weak interactions result in a 2-D double layer conformation where the uncoordinated perchlorate anions are inserted in the packing space and take part in the H-bond interactions, and each complex is connected with six neighboring complexes and three perchlorate anions.     

Solvothermal Synthesis,Crystal Structure and Photoluminescent Property of a Novel 3D [Ca2（HCOO）2（nds）（H2O）2]n

A novel calcium（Ⅱ） metal-organic framework [Ca2（HCOO）2（nds）（H2O）2]n（1） with mixed 1,5-naphthalenedisulfonate sodium salt（1,5-nds） and formate as organic ligands has been obtained under solvothermal conditions.It was found that theμ3-η2∶η2 bridging mode of HCOO-in compound 1 is uncommon.Moreover,the formate,which was in situ formed from N,N＇-dimethylformamide,played an important role in the formation of 3D structure.HCOO-ligands bridged Ca（Ⅱ） ions into grid-like layers that were further pillared by the 1,5-nds ligand to form a 3D Ca-based framework.Compound 1 also exhibits a strong blue luminescence at room temperature.     

Synthesis and Crystal Structure of Complex [Pb(qina)_2(DMSO)]·H_2O

A novel complex [Pb(qina)2(DMSO)]·H2O was synthesized,of which qina-is the quinaldic acid radical and DMSO the dimethyl sulfoxide. Elemental analysis,IR spectra,and X-ray single-crystal diffraction were carried out to determine the composition and crystal structure. This complex belongs to monoclinic system,space group P121/n1,with a=7.1553(17),b=17.543(2),c=17.306(2) ,β=91.671(4)°,C22H20N2O6PbS,Mr=647.65,Z=4,V=2171.5(6) 3,Dc=1.981 g/cm3,μ=7.908 mm-1,F(000)=1248,–9≤h≤6,–23≤k≤19,–22≤l≤22,R=0.0221 and wR= 0.0488. Weak coordinate bond is formed between oxygen atom in DMSO and Pb(Ⅱ ) . There are also weak interactions,such as π-π interaction,hydrogen bonds and so on,among the complex molecules.     

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.     

新型—维锯齿链状聚金属氧酸盐配位聚合物［｛La(DMSO)_6(H_2O)}·(PMo_(12)O_(40))·H_2O］_n的合成、结构及表征

以a-H_3PMo_(12)O_(40)·nH_2O, La_2O_3和二甲基亚砜（DMSO）为原料，在 乙腈和水的混合溶剂中制得了一维锯齿链状配位聚合物［｛La(DMSO)_6(H_2O)}· (PMo_(12)O_(40))·H_2O］_n,X射线单晶衍射结果表明，聚合物中金属配阳离子与 杂多阴离子骨架通过Mo-O_d-La-O_d-Mo相连并形成一维无限链，每一个不对称结构 单元中含一个结晶水，La~(3+)的配位数为九，三帽三棱柱构型，配位氧原子分别 来自6个DMSO分子，1个H_2O分子和2个相邻杂多阴离子的端氧，晶体氧于单斜晶系 ，P2_1/c空间群，a=1.3916(3)nm,b=1.7058(3)nm,c=2.4750(5)nm,β=99.16(3)~° ,Z=4,V=5.800(2)nm~3,D_c=2.825g/cm~3,R_1=0.0446,wR_2=0.0871,IR光谱和X射线 单晶衍射结果一致表明，在固态条件下配阳离子和杂多阴离子之间存在相互作用， UV光谱表明，在稀的水溶液中，由于溶剂化作用，杂多阴离子与配阳离子处于解离 状态，热性质研究表明，形成标题化合物后，杂多阴离子的热稳定性与磷钼酸相比 明显增强。     

铋配合物[Bi(S2CNC5H10)2(NO3)]·[1，10-Phen]·0.5H2O的合成及晶体结构

The bismuth complex with dithiopiperdylcarbamate [Bi(S₂CNC₅H₁₀)₂(NO₃)]·[1，10-Phen]·0.5H₂O was synthesized. The crystal and molecular structure were determined by X-ray single crystal diffraction. The crystal belongs to monoiclinic with space group C2/c, a=3.140(2) nm, b=1.176 4(9) nm, c=2.021 6(15) nm, β=103.081(12)°, V=5.713(7) nm³, Z=8, F(000)=3064, D_c=1.815 g·cm^-3, μ=6.502mm^-1. The final R₁=0.0332, wR₂=0.040 3. In the complex, the bismuth atom is eight-coordinated in a capped distorted pentagonal bipyramidal geometry. CCDC: 222655.     

Synthesis and Structure of a POMs-based 3D Zeolike Ionic Crystal, {[Co（dpdo）2（H2O）2（CH3CN）]2（SiMo12O40）（H2O）2}n

A POMs-based 3D zeolike ionic crystal 1, {[Co（dpdo）2（CH3CN）（H2O）2]2（SiMo12O40）- （HEO）2}n （dpdo = 4,4＇-bipyridine-N,N＇-dioxide）, was constructed via self-assembly by embedding Keggintype [SiMo12O40]^4- polyanions within the intercrystalline voids as pillars and structurally characterized. The crystal structure was determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P1 with a = 11.430（3）, b = 12.242（3）, c = 14.279（3）A, α = 106.196（4）,β = 94.316（4）, γ = 98.294（3）°, V = 1884.5（7）A^3 Z = 1, C44H50N10O54CoEMo12Si, Mr = 2880.17, Dc = 2.538 g/cm^3, p = 2.484 mm^-1,F（000） = 1388, the final R = 0.0383 and wR = 0.1096 for 7753 observed reflections with I 〉 2σ（I）. Flack factor is 0.22（3）. Compound 1 is a pillar-layered framework with the [SiMo12O40]^4- anions linearly located on the square voids between the 2D bilayers which are formed by the dpdo ligands and cobalt（II） ions.     

桥联双核配合物[(DPC)2Co2(H2O)5]·2H2O的合成与晶体结构

The new complex formulated [(DPC)₂Co₂(H₂O)₅]·2H₂O (HDPC^- is pyridine-2,6-dicarboxylate) has been synthesized and the crystal structure was determined by X-ray diffraction. The crystal structure of the complex belongs to monoclinic system with space group P2₁/c, a=0.83850(10) nm, b=2.7386(4) nm, c=0.9610(2) nm, β=98.280 (10) °, V=2.1838(6) nm³, Z=4, D_c=1.746 g·cm^-3, μ=1.597 mm^-1. In the crystal the two Co²⁺ are in distorted octahedrons. The part of [Co(DPC)₂] possess an approximate D_2d symmetry, while the part of [OCo₍₂₎(OH₂)₅] has an approximate C₂ symmetry.     

Synthesis and Crystal Structure of Complex: [Co(cdm)_2(H_2O)_4].2H_2O (cdm=Carbamyldicyanomethanide Anion)

1 INTRODUCTION Crystal engineering and the design of solid-state architectures have recently become areas of increasing interest[1, 2]. Such crystal engineering may afford new materials with useful properties such as catalytic activity, micro-porosity, nonlinear optical activity, cooperative magnetic behavior and so on. Polynitrile-ligand is one of the ideal multi-functional ligands for crystal engineering and many complexes with polynitriles as ligands have been found to show the spe…     

Synthesis,Crystal Structure and Quantum Chemistry of the Complex [Cu（p-FBA）_2（phen）（H_2O）]

A novel metal-organic complex Cu(p-FBA)2(phen)(H2O) (p-FBA = p-fluorobenzoic acid,phen = 1,10-phenanthroline) has been synthesized and structurally characterized by X-ray single-crystal diffraction,elemental analysis and IR spectra. The crystal belongs to triclinic,space group P1 with a = 7.8043(7),b = 10.4069(9),c = 14.3658(13) ,α = 105.3170(10),β = 96.877(2),γ = 96.7580(10)o,V = 1103.56(17) 3,Mr = 539.96,Z = 2,Dc = 1.625 g/cm3,μ = 1.050 mm-1,F(000) = 550,the final R = 0.0324 and wR = 0.0952. In the crystal,the structure consists of discrete molecules containing a five-coordinate copper(Ⅱ ) in a distorted square pyramidal configuration. Intramolecular O-H···O hydrogen bonds,weak intermolecular C-H···O hydrogen bonds and π-π stacking link the molecules into a one-dimensional chain structure. The study on the title complex has been performed with quantum chemistry calculation by means of G03W package on the Lanl2dz basis set. The stabilities of the complex together with the orbital energies and composition characteristics of some frontier molecular orbitals have been investigated.