Syntheses and Structures of Lanthanide Complexes with Isonicotinate

1 INTRODUCTION In recent years, chemists have paid their attention to the design and construction of extended metal- organic framework solids with potential applications, such as catalysts, nonlinear optical devices, ion ex- change, adsorption, sensors etc.[1, 2]. As one kind of polydentate ligands, isonicotinic acid has been exte- nsively employed to synthesize transition metal coo- rdination polymers[3, 4] with one-[5～8], two-[9～12] and three- dimensional[13～21] extended frameworks b…     

Syntheses and Crystal Structures of [Ni(L)2(NCS)2] and [Co(L)2(NCS)2] (L = Azobis(2-pyridine)

1 INTRODUCTION The synthesis of new organic-inorganic hybrid compounds is a relatively new research area that has developed rapidly in the last several years[1]. Bische- late ligand[2, 3], such as azobis(2-pyridine), is a novel tetradentate ligand expect…     

Syntheses and Crystal Structures of Two Cyano-bridged Bimetallic Complexes [Ln(DMSO)2(H2O)(μ-CN)4Fe(CN)2](Ln= Ce and Eu, DMSO= Dimethylsulfoxide) with Layered Structure

Two new bimetallic cyano-bridged complexes [Ln(DMSO)2(H2O)(μ-CN)4Fe(CN)2] (Ln = Ce 1, Eu 2) have been prepared by the grinding reaction method and structurally characterized by X-ray single-crystal structure analysis. Crystallographic data for 1: C10H14CeFeN6O3S2, Mr = 526.36, monoclinic, P2/n, a = 7.852(4), b = 10.729(5), c = 11.181(5) (A), β = 96.992(8)°, V = 935.0(7) A3, Z = 2, Dc = 1.870 g/cm3, μ = 3.421 mm-1, F(000) = 512, R = 0.0363 and wR = 0.0971; and those for 2: C10H14EuFeN6O3S2, Mr = 538.20, monoclinic, P2/n, a = 7.739(5), b = 10.668(7), c = 11.008(7) A, β = 96.943(3)°, V = 902.1(11) A3, Z = 2, Dc = 1.981 g/cm3, μ= 4.499 mm-1, F(000) = 522, R = 0.0345 and wR = 0.0855. In each complex the lanthanide ion is seven-coordinated in a pentagonal bipyramidal arrangement, and the Fe(Ⅲ) ion is in a nearly regular octahedral environment. The title complexes can be described as two-dimensional (2-D) stair-like structures, which are further connected by hydrogen bonds to form three-dimensional (3-D) frameworks.     

Syntheses and Crystal Structures of Two One-dimensional Coordination Polymers Constructed from a Flexible Hinge-like Ligand

By using the flexible hinge-like ligand 2,2＇-bis（3-hydroxy-l,4-naphthoquinone） （H2bhnq）, two isomorphous one-dimensional zigzag chain coordination polymers have been obtained. Single-crystal X-ray analyses revealed that the metal centers in these two complexes are distorted octahedra involving four oxygen atoms of two bhnq2 anions, and two oxygen atoms of two DMF molecules situated in trans positions to one another. Crystal data for [Mn（bhnq）（DMF）2]n 1： C26H22MnN2O8, Mr = 545.40, monoclinic, space group C2/c, a = 14.936（3）, b = 10.362（2）, c = 15.901（3）A., β = 99.86（3）°, V = 2424.7（8）A3, Z = 4, Dc = 1.494 g/cm^3, F（000） = 1124,μ = 0.599 mm^-1, final GOOF = 1.025, R = 0.0654 and wR = 0.1537. Crystal data for [Cd（bhnq）（DMF）2]n 2： C26H22CdN2O8, Mr = 602.86, monoclinic, space group C2/c, a = 14.839（3）, b = 10.493（2）, c = 16.034（3）A, β = 99.40（3）°, V = 2463.1（9）A^3, Z = 4, Dc = 1.626 g/cm^3, F（000） = 1216,μ = 0.941 mm^-1, final GOOF = 1.069, R = 0.0358 and wR = 0.0944.     

Two Novel Zinc Compounds with in situ Formation of Dimethylamine Ligand

The investigation of the supramolecular interactions between the zinc chloride salts and the crown ether in tetrahydrofuran （THF） with the diffusion of in situ formed DMA （DMA = dimethylamine） ligand leads to two novel zinc-DMA compounds, [（H3O）·（18C-6）][ZnCl3（DMA）] 1 and [（HDMA）·（18C-6）][ZnCl3（DMA）] 2 （18C-6 = 18-crown-6）, whose emissions fall into the blue-emission field. Crystal data for compound 1： monoclinic, space group P21/c, a = 8.753（1）, b = 14.538（2）, c = 19.969（3）A, β = 110.121（7）°, V = 2386.2（5）A^3, T = 293（2） K, Z = 4, Mr = 500.14, Dc= 1.392 g/cm^3,μ = 1.395 mm^-1, F（000） = 1048, S = 1.006, R = 0.0611 and wR = 0.1755 for 3676 observed reflections with I 〉 2σ（I） and 235 parameters. For 2： triclinic, space group P1^-, a = 9.2672（4）, b = 11.8778（2）, c = 13.3846（1） A, a = 67.09（1）, β = 75.54（2）, ）,γ = 81.32（2）°, V = 1311.74（6） A^3, T = 293（2） K, Z = 2, Mr = 527.21, Dc = 1.335 g/cm^3,μ = 1.271 mm^-1, F（000） = 556, S = 1.006, R = 0.0393 and wR = 0.1034 for 3839 observed reflections with I〉 2σ（I）.     

Syntheses and Crystal Structures of 4-Amino-3- （3-hyd roxyp ropyl）- 1H-1,2,4-triazole-5（4H）-thione and 6-（4-Biphenylyl）-3-（3-hydroxypropyl）-7H-1,2,4-triazolo[3,4-b][1,3,4]thiadiazine

1INTRODUCTION It has been reported that3,6-disubstituted-7H-1,2,4-triazolo[3,4-b][1,3,4]thiadiazines have a broad spec-trum of bioactivities,such as antimicrobial[1],antibac-terial,antifungal[2],anti-inflammatory[3],diuretic[4],an-thelmintic and analgesic[5].They can also be used as plant-growth regulating agents[6],photographic coup-lers,dyes for improved preservability and absorption characteristics,and inhibitors of malignant cellularZOU K.H.et al.:Syntheses and Crystal Structures o…     

Syntheses and Crystal Structures of Two Complexes with 3-（3-Pyridyl）acrylic Acid

1 INTRODUCTION A recent feature in the development and progress of chemical research is the concern for molecular assemblies, ensembles, and all of structural aggre- gates[1]. The self-assembly of transition metal ions and N-containing organic ligands has been proven a popular approach for the construction of supramo- lecular architecture[2～7]. 3-(3-Pyridyl)acrylic acid is an excellent ligand, not only due to its prolific coor- dination sites but also to its potential hydrogen bon- ding…     

Syntheses and Crystal Structures of Two Novel Cobalt(Ⅱ) Complexes with 2-Amino-5-substituted-1,3,4-thiadiazole as Ligands

Two novel cobalt(Ⅱ) compounds were obtained and characterized by X-ray single-crystal diffraction,IR,1H NMR and elemental analysis.Compound 1 crystallizes in monoclinic,space group P21/n,with a = 18.046(4),b = 11.335(3),c = 19.157(5) ,β = 92.707(3)o,Z = 4,V = 3914.4(16) 3,Mr = 968.56,Dc = 1.644 g/cm3,μ = 1.378 mm-1,F(000) = 1960,the final R = 0.0367 and wR = 0.0895.The crystal of compound 2 is of monoclinic,space group P21/c with a = 8.7253(10),b = 10.9031(13),c = 18.235(2) ,β = 93.2210(10)o,Z = 4,V = 1732.0(3) 3,Mr = 464.21,Dc = 1.780 g/cm3,μ = 1.560 mm-1,F(000) = 932,the final R = 0.0322 and wR = 0.0743.     

Synthesis and Crystal Structure of 2-（N-Cyclohexyl）-imino-1,4-succinic Acid Dihydrate

1INTRODUCTIONItiswellknownthatthetwentyα-aminoacidsarethemostcommononesexistinginnature[1,.2]Actually,nineteenα-aminoacidsandoneα-iminoacidareutilizedinlivingcellsforproteinsynthesisunderthecontrolofgenes.Theyareinaspecialca-tegoryduetotheirfundamentalsofalllifeformsasbuildingblocksforlifeproteins[3～5].Aminoacidsarealsoimportantnaturalchiralmaterialsforsyn-thesizingpeptides,alkaloids,antibioticandmorecomplexmoleculeswithbiologicalactivities[6].Ac-cordingtothesyntheticmethodology,amino…     

Solvothermal Syntheses and Crystal Structures of Two New Nonmetal Borates: C4H10N2·B6O8(OH)2 and (NH3CH2CH2NH3)B5O8(OH)

Two new borate compounds, C4H10N2·B6O8(OH)2 1 and (NH3CH2CH2NH3)B5O8(OH)2, have been solvothermally synthesized and structurally characterized by single-crystal X-ray diffraction, IR, elemental analysis and thermal analysis. Compound 1 crystallizes in the monoclinic system, space group P21/c, with a = 8.3318(17), b = 6.2118(12), c = 12.479(3) (A), β = 108.96(3)°, V = 610.8(2) (A)3, Mr = 313.02, Z = 2, Dc= 1.702 g/cm3, μ = 0.150 mm-1, F(000) = 320, R = 0.0387and wR = 0.0924. Its layered structure is linked by infinite covalently coordinated neutral sheets with 3,20-membered window system, which are built up from alternative B6O8(OH)2 subunits donated by two piperzazine nitrogen donors. 2 crystallizes in monoclinic, space group Cc, with a =6.7207(13), b = 11.481(2), c = 12.564(3) (A),β = 95.25(3)°, V= 965.4(3) (A)3, Mr= 261.18, Z= 4, Dc=1.797 g/cm3, μ = 0.164 mm-1, F(000) = 536, R = 0.0396 and wR = 0.0752. Its oxoborate structure is generated from the sheets of 3,9-membered boron rings bonded diamine molecules through electrostatic and H-bonding interactions to form a two-dimensional layered network.     

Supramolecular Formation via Hydrogen Bonding in Copper and Nickel Complexes with 2-Hydroxynicotinic Acid

Two complexes,Cu(HnicO)2 1 and Ni(HnicO)2(H2O)2 2 (H2nicO=2-hydroxy-nicolinic acid),were synthesized by hydrothermal reactions and structurally characterized. Complex 1 crystallizes in monoclinic,space group P21/n,with a=8.314(7),b=6.275(4),c=11.283(7),β =98.32(3)°,V=582.5(7)3,Z=2,Mr=339.74,Dc=1.937 g/cm3,F(000)=342,μ=1.908 mm-1,S =1.097,the final R=0.0284 and wR=0.0781 for 1177 observed reflections with I > 2σ(I). Complex 2 crystallizes in monoclinic,space group P21/c,with a=7.438(5),b=12.22(1),c=7.537(5),β=100.07(3)°,V=674.3(8)3,Z=2,Mr=370.95,Dc=1.827 g/cm3,F(000)=380,μ =1.487 mm-1,S=1.041,the final R=0.0335 and wR=0.0779 for 1202 observed reflections with I > 2σ(I). There are extended 3D framework structures in complexes 1 and 2 due to the N–H…O and C–H…O hydrogen bonds. The copper atom in 1 has square planar coordination,while the nickel atom in 2 adopts octahedral coordination geometry. The TG curve shows that complex 2 is stable in solid state to 150 ℃.     

Synthesis and Structural Characterization of One New Polyoxotungstate Connected via Potassium Cations with a Three-dimensional Framework: H6Na2K4(H2W12O42)Cl2·14H2O

One new polyoxotungstate complex H6Na2K4(H2W12O42)Cl2·14H2O 1 has been prepared in the beaker solution and characterized by elemental analysis and IR spectroscopy. Crystal data: H36Cl2K4W12Na2O56, Mr = 3411.77, monoclinic, space group P21/c, a = 11.5734(16), b = 14.3136(19), c = 15.459(2)(A), β = 105.601(2)°, V = 2466.5(6)(A)3, Z = 2, Dc = 4.594 g/cm3, F(000) = 3008, μ = 28.447 mm-1, R = 0.0574 and wR = 0.1239 (Ⅰ＞ 2σ(Ⅰ)). Single-crystal X-ray diffraction analysis results reveal that a three-dimensional architecture in the title compound is constructed from the H2W12O4210- units linked by potassium.     

Syntheses and Crystal Structures of Two Coordination Polymers with Aromatic Dioxide as Bridge Ligands

Two coordination polymers, namely, two-dimensional complex 1 {[Cu(μ- L)1.5(ClO4)2(H2O)].(H2O)0.5}n (L = pyrazine-1,4-dioxide) and one-dimensional complex 2 [Co(μ-L)Br2(H2O)2]n, have been synthesized with pyrazine-1,4-dioxide as bridging ligands, and their crystal structures were determined by X-ray crystallography. Crystal data for complex 1: monoclinic system, space group C2/c, with a = 23.310(3), b = 12.2338(17), c = 10.6075(15) , β = 110.487(2)°, V = 2833.6(7) 3, Z = 8, C6H9Cl2CuN3O12.5, Mr = 457.60, Dc = 2.145 g/cm3, F(000) = 1832 and μ = 1.998 mm-1; and those for 2: monoclinic system, space group C2/c, with a = 11.012(3), b = 7.483(2), c = 11.451(3) , β = 101.654(4)°, V = 924.2(4) 3, Z = 4, C4H8Br2CoN2O4, Mr = 366.87, Dc = 2.637 g/cm3, F(000) = 700 and μ = 10.487 mm-1. 1 shows a two-dimensional sheet structure on the ac plane through the coordination of μ-L bridging ligands with Cu(II) ions, while 2 displays a zigzag one-dimensional chain along the c axis via the coordination of μ-L bridging ligand with Co(II) ions. Hydrogen bonds in 1 and 2 make the sheets (or chains) connect each other to form a three-dimensional structure.     

Zero- and One-dimensional Organic-inorganic Hybrid Compounds Based on Monovacant Keggin Polyoxotungstatesa

Two new organic-inorganic hybrid mono-transition-metal-substituted polyoxometalates [Ni(2,2'-bipy)3]3[Ni(H2O)SiW11O39]·11H2O 1 and [Cu(dien)(H2O)][Cu(dien)(H2O)2]2-[CuSiW11O39]·5.5H2O 2 (2,2'-bipy = 2,2'-bipyridine, dien = diethylenetriamine) have been hydrothermally synthesized and characterized by single-crystal X-ray diffraction, elemental analysis, magnetic properties, and IR spectrum. Crystal data for 1: monoclinic, space group P21/n, a = 17.492(3), b = 33.481(5), c = 20.493(3) A, β = 101.894(3)°, Dc = 2.563 mg/A3, F(000) = 8440,μ = 11.454 mm-1 and Z = 4; and those for 2: monoclinic, space group P21/n, a = 11.114(3), b = 22.803(7), c = 22.468(7) A, β = 97.896(6)°, Dc = 4.036 mg/A3, F(000) = 6140,μ = 23.942 mm-1 and Z = 4. The study on the magnetic susceptibility of 2 demonstrates the presence of ferromagnetic interaction.     

Syntheses, Crystal Structures and Fluorescence Properties of Two Pb（II） 1-Naphthoate Complexes

Two new 1-naphthoate-based Pb(Ⅱ) complexes, [Pb(phen)(NA)2]n 1 and [Pb(bpp)(NA)2]n 2 (NA = 1-naphthoate, phen = 1,10-phenanthroline, and bpp = 1,3-bi(4-pyri- dyl)propane), were hydrothermally synthesized and structurally characterized. 1 is of monoclinic system, space group C2/c with a = 28.114(3), b = 10.9601(10), c = 8.6843(8) , β = 93.3760(10)°, V = 2671.3(4) 3, Dc = 1.814 g/cm3, Mr = 729.73, Z = 4, F(000) = 1416, μ = 6.360 mm-1, the final R = 0.0346 and wR = 0.0948 for 2184 observed reflections with I > 2σ(I). Complex 2 crystallizes in monoclinic, space group C2/c with a = 26.491(2), b = 8.7773(6), c = 27.893(2) , β = 113.3020(10)°, V = 5956.8(8)3, Dc = 1.668 g/cm3, Mr = 747.78, Z = 8, F(000) = 2928, μ = 5.706 mm-1, the final R = 0.0211 and wR = 0.0493 for 3677 observed reflections with I > 2σ(I). Both complexes present one-dimensional (1-D) zigzag chains extended by anionic NA linkers for 1 and bridged by neutral bpp connectors for 2, which are further aggregated into 2-D supramolecular networks by interchain π···π stacking interactions. In addition, the two solid-state complexes exhibit different strong emissions at room temperature, suggesting their potential applications as fluorescence materials.     

Syntheses and Crystal Structures of Two 3D Zinc(II) Compounds Involving Coordination and Hydrogen Bonds

1 INTRODUCTION Self-assembly through coordination and hydrogen bonds has been proved to be a powerful tool for con- structing functional organic crystalline materials[1~4]. Except for the important role of H-bonds in the sta- bilization of structures, hydrogen bonding groups namely hydroxyl, amide groups in adjacent coor- dination polymeric chains or discrete lamellas can form hydrogen bonds, which allow for the assembly of well-formed crystalline solid[5, 6]. Our recent inte- rest is foc…     

Template Syntheses and Crystal Structures of Hexaaza Macrocyclic Complexes with C-Methyl Substituents

1 INTRODUCTION Polyaza-macrocyclic compounds with functional substituents have been extensively investigated recen- tly because of their potential applications in radioac- tive therapy, recovery of metal ions, biomimetic che- mistry, and catalysis[1, 2]. With various structures and distinctive properties, they have become significant building blocks for further chemical studies[3～6]. As far as the preparation method is concerned, metal template condensation reactions are shown to be effec…     

Synthesis and Crystal Structure of 4-Bromo-5-ethoxy-3-methyl-5- （naphthalen- 1-yl）- 1-tosyl- 1H-pyrrol-2（5H）- one

The title compound 4-bromo-5-ethoxy-3-methyl-5-(naphthalen-1-yl)-1-tosyl-1H- pyrrol-2(5H)-one 1 (C24H22BrNO4S, Mr = 500.40) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in monoclinic, space group P21/n with a = 8.8562(15), b = 18.118(3), c = 14.055(2) , β = 99.855(3)o, V = 2221.9(6) 3, Z = 4, Dc = 1.496 g/cm3, μ = 1.975 mm-1, λ = 0.71073 , F(000) = 1024, R = 0.0607 and wR = 0.1371.     

Synthesis and Structural Characterization of a Polyoxomolybdate HNa7[Mo36O112(H2O)16]·47H2O

A new polyoxomolybdate complex HNa7[Mo36O112(H2O)16]·47H2O 1 has been prepared in the beaker solution and characterized by single-crystal X-ray diffraction and elemental analyses. Crystal data: H127Mo36Na7O175, Mr = 6542.79, monoclinic, C2/c, a = 40.891(6), b =17.900(3), c = 25.580(4) (A), β = 125.673(2)°, V = 15210(4)(A)3, Z = 4, Dc = 2.857 g/cm3, F(000) =12464, μ = 3.013 mm-1, R = 0.0633 and wR = 0.1654 (I＞ 2σ(Ⅰ)). With the bridging sodium cations,the [Mo36O112(H2O)16]8- units in compound 1 are linked to form a one-dimensional structure, on the basis of which a three-dimensional architecture is further constructed via other sodium cations and complicated hydrogen bonds.     

Syntheses and Crystal Structures of Two New Iron-sulfur Carbonyl Complexes: [Fe2(SC6H4Cl)2(CO)6]·0.5(Et2O) and [Fe3(SC6H4NH2)6(CO)6]·2(MeOH)

Two new iron-sulfur carbonyl complexes, [Fe2(SC6H4Cl)2(CO)6]·0.5(Et2O) 1 and [Fe3(SC6H4NH2)6(CO)6]·2(MeOH) 2, have been prepared and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. Crystal data for 1: monoclinic, C2/c, a = 18.4439(8), b = 11.0999(5), c = 25.1830(10)(A), β = 97.0370(10)o, V = 5116.8(4)(A)3, Z = 8, C20H13Cl2Fe2O6.50S2, Mr = 604.02, Dc = 1.568 g/cm3, μ = 1.540 mm-1, F(000) = 2424, the final R = 0.0545 and wR = 0.1454 for 3443 observed reflections with I > 2σ(I); 2: monoclinic, P21/n, a = 12.350, b = 26.3050(11), c = 16.057(A),β = 97.891(3)°, V = 5166.9(2)(A)3, Z = 4, C44H44Fe3N6O8S6, Mr = 1144.76, Dc = 1.472 g/cm3, μ = 1.128 mm-1, F(000) = 2352, the final R = 0.0442 and wR = 0.1197 for 7978 observed reflections with I > 2σ(I). Complex 1 contains one iron dimer, in which two tricarbonyliron(I) fragments are bridged together by two 4-chlorophenylthiolate ligands, whereas complex 2 contains a linear tri-iron cluster, in which two terminal tricarbonyliron(II) fragments and the central Fe(II) atom are linked together by six 4-aminophenylthiolate bridging ligands.