Synthesis,Structure and Luminescent Property of a New bnn-type Zn(Ⅱ) Coordination Polymer

A new Zn(Ⅱ) coordination polymer, namely [Zn(Htci)(bib)0.5(H2O)]n·nH2O(1, H3 tci = tri(2-carboxyethyl)isocyanurate, bib = 1,4-bis(imidazol-1-ylmethyl)-butane) has been synthesized by combining H3 tci and bib ligands with Zn(Ⅱ) salts under solvothermal conditions. The title compound crystallizes in monoclinic, space group P21/c with a = 13.3424(7), b = 7.9051(5), c = 20.4650(12) , β = 101.935(5)o, V = 2111.8(2) 3, C17H24N5O11 Zn, Mr = 539.8, Z = 4, Dc = 1.698 g/cm3, F(000) = 1116, μ = 1.236 mm-1, the final R = 0.0398 and wR = 0.00879 for 3722 observed reflections(I 2■(I)). X-ray structural analysis reveals that compound 1 exhibits a three-dimensional(3D) pillar-layered framework, and can be simplified into a 5-connected bnn topological network. Moreover, the luminescent properties for compound 1 were also studied at room temperature.     

A Zn(II) 5-Aminoisophthalate Coordination Polymer

The title compound, [Zn(AIP)(4,4-bipy)0.5(H2O)]n·0.75nH2O 1, was synthesized via the hydrothermal reaction of Zn(OAc)2 with 5-aminoisophthalic acid (H2AIP) and characterized by elemental analysis and infrared spectra. The complex crystallizes in monoclinic system, space group P21/c with a = 12.672(1), b = 7.6557(4), c = 16.181(1) , β = 109.187(2)o, V = 1482.6(2) 3, Z = 1, C52H52N8O23Zn4, Mr = 1418.58, Dc = 1.589 g/cm3, F(000) = 724 and μ(MoKα) = 1.685mm-1. The final R = 0.0702 and wR = 0.1524 for 1847 observed reflections with I > 2σ(I), and R = 0.0873 and wR = 0.1664 for all data. X-ray diffraction studies reveal that the title compound has an interesting 2D microporous architecture with guest water molecules inside the channel.     

Synthesis and Structure of a Zinc(II) Complex:[Zn(Pybta)·Cl_2]_n

The title compound, [Zn(Pybta)Cl2]n (Pybta = 1-(2-pyridylmethyl)benzontriazole), has a zigzag chain structure. It crystallizes in the monoclinic system, space group P21/c with a = 9.0103(11), b = 17.0276(18), c = 9.2288(11) , β = 101.309(6)o, Mr = 346.51, V = 1388.4(3) 3, Z = 4, Dc = 1.658 g/cm3, F(000) = 696, μ = 2.143 mm1, the final R = 0.0492 and wR = 0.1236 for 2545 observed reflections with I > 2σ(I). The Zn atom is four-coordinated by two N and two Cl atoms, forming a slightly distorted tetrahedral geometry. Each zigzag chain links its adjacent symmetry- related equivalents via multiple π-π interactions, which are not frequently observed in the previously reported architectures.     

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 Structural Characterization of a Polyoxomolybdate HNa_7[Mo_(36)O_(112)(H_2O)_(16)]·47H_2O

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) , β = 125.673(2)°, V = 15210(4) 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.     

Synthesis and Crystal Structure of a Copper(Ⅱ) Compound with 4-Hydroxybenzoic Acid and Isonicotinamide:[Cu(4-hba)_2(inta)(H_2O)]·H_2O

A new copper(Ⅱ) compound has been prepared and fully characterized by elemen-tal analysis,IR,TG and single-crystal X-ray diffraction.The compound [Cu(4-hba)2(inta)(H2O)]·H2O (4-hba=4-hydroxybenzoic acid,inta=isonicotinamide) 1 crystallizes in the monoclinic system,space group P21/c with a=7.590(5),b=11.027(5),c=23.761(5),β=102.5740(10)o,V=1974.1(16) 3,Mr=991.84,Z=2,Dc=1.669 g/cm3,F(000)=1020,μ=1.166 mm-1,R=0.0353 and wR=0.0604 for 3166 observed reflections (I 2σ(I)).In compound 1,the copper cation is penta-coordinated with two carboxylate oxygen atoms from two different 4-hba ligands,two oxygen atoms from two coordinated water molecules and one nitrogen atom from inta ligand,showing a slightly distorted square-pyramidal geometry.     

Hydrothermal Synthesis,Crystal Structure and Fluorescent Property of a Novel Polyoxometalate [H_6Mo_8~(VI)O_(27)]·3C_4N_2H_(10)

A new infinite three-dimensional framework structure of the title compound [H6MoVI8O27]·3C4N2H10 has been synthesized under mild hydrothermal conditions and charac-terized by elemental analyses,IR,fluorescent spectra and single-crystal X-ray diffraction.C12H36Mo8N6O27 crystallizes in the triclinic system,space group P 1 with a = 8.820(3),b = 9.534(3),c = 10.993(4) ,α = 99.985(17),β = 106.65(2),γ = 101.650(14)o,V = 840.6(5) 3,Mr = 1463.99,Z = 1,Dc = 2.892 g/cm3,μ = 2.993 mm-1,F(000) = 702,the final R = 0.0676,wR = 0.1920 and S = 1.074 for 2196 observed reflections with I > 2σ(I).The title compound exhibits a novel infinite three-dimensional(3D) framework composed of a [H6MoVI8O27] subunit and three dissociated piperazine fragments.The complex exhibits two strong fluorescent emission bands at ca.417 and 440 nm(λex = 378 nm) in the solid state at room temperature.     

Synthesis and Crystal Structure of Dimethyl-3-（4-bromophenyl）-1-phenyl-4,5-dihydro-1H-pyrazole-4,5-dicarboxylate

The title compound (C19H17BrN2O4) was synthesized via a one-pot procedure starting from 4-bromobenzaldehyde, dimethyl acetylenedicarboxylate (DMAD) and phenylhydrazine with pyridine as the catalyst. Its structure was determined by single-crystal X-ray diffraction analysis. The crystal belongs to the monoclinic system, space group P21/c with a = 11.115(3), b = 8.090(2), c = 20.211(5) , β = 97.032(5)°, V = 1803.7(8) 3, Z = 4, Mr = 417.25, Dc = 1.536 g/cm3, μ = 2.306 mm-1, F(000) = 852, the final R = 0.0403 and wR = 0.0895 for 2215 observed reflections with I 2σ(I).     

Addition Reaction of Bis（diphenylphosphinyl） Butadiyne with Methylcyclopentadiene

Bis(diphenylphosphinyl)butadiyne reacted with methylcyclopentadiene at room tem- perature and four isomeric products were obtained. Crystal structures of isomers 1 and 3 have been determined. Crystal data for compound 1 C40H36O2P2·2CHCl3: monoclinic, space group C12/c1 with a = 17.983(2), b = 11.8723(12), c = 20.081(2) , β = 111.218(3)°, V = 3996.5(8) 3, Z = 4, Mr = 849.36, Dc = 1.412 g/cm3, F(000) = 1752, μ = 0.546 mm-1, the final R = 0.0351 and wR = 0.0951 for 3965 observed reflections (I > 2σ(I)); and those for compound 3 C40H36O2P2·H2O: triclinic, space group P1 with a = 10.4144(15), b = 13.0558(18), c = 13.742(2) , α = 70.453(8), β = 75.382(8), γ = 72.312(8)°, V = 1653.7(4) 3, Z = 2, Mr = 628.64, Dc = 1.262 g/cm3, F(000) = 664, μ = 0.169 mm-1, the final R = 0.0593 and wR = 0.1296 for 4891 observed reflections (I > 2σ(I)). The structures of the other two isomers are identified via IR, 1H NMR and MS spectra.     

Synthesis and Crystal Structure of N-Phenylbis（ferrocenecarboxyl）imide

The ferrocenyl compound,N-phenylbis(ferrocenecarboxyl)imide (C28H23NO2Fe2,Mr=517.17),was synthesized and structurally characterized by means of X-ray single-crystal dif-fraction. It crystallizes in monoclinic,space group C2/c with a=21.374(14),b=10.430(7),c= 10.741(7) ,β=114.184(8)°,V=2184(2) 3,Z=4,Dc=1.573 g/cm3,F(000)=1064,μ(MoKα)= 1.355 mm–1,T=291(2) K,the final R=0.0548 and wR=0.1437 for 1524 observed reflections with I > 2σ(I). In this compound,the nitrogen atom links two ferrocenyl groups and one phenyl group forming a novel imido derivative.     

Blue Luminescent Zinc(Ⅱ)- and Cadmium(Ⅱ)-1,4-phenylenediacetate Complexes

Two mixed-ligand polymeric complexes formulated as {[Zn(pda)(bpy)]·0.5H2O}n (pdathermally synthesized. Single-crystal X-ray diffraction analyses reveal that the structures of complexes 1 and 2 possess similar one-dimensional zigzag chains. Crystal data for compound 1: monoclinic, space group P21/c, a = 15.965(2), b = 8.305(1), c = 14.856(2) (A),β= 1 1 1.048(2)°, Mr = 422.73, V= 1838.2(4) A3, Z= 4, Dc = 1.528 g/cm3, μ = 1.368 mm-1, F(000) = 868, the final R = 0.0783 and wR= 0.1469 (w=1/[σ2(Fo2) + (0.035 1p)2+ 8.0014P], where P = (Fo2+ 2Fc2)/3) based on 2025 observed reflections with I ＞ 2σ(I); and those for compound 2: monoclinic, space group C2/c, a = 29.921 (7), b= 8.5400(17), c = 15.320(3) (A),β= 99.59(3)°, Mr = 487.75, V = 3859.9(14) A3, Z = 8, Dc = 1.668g/cm3, μ = 1.169 mm-1, F(000) = 1936, the final R = 0.0723 and wR = 0.1612 (w = 1/[σ32(Fo2 ) +(0.0681p)2+ 55.9577P], where P = (Fo2+ 2Fc2)/3) based on 2130 observed reflections with I ＞ 2σ(I).Fluorescent analyses show that both complexes exhibit intense blue luminescence (λmax = 485 nm for 1and 475 nm for 2) upon excitation at 330 nm.     

Syntheses and Crystal Structures of Two New Organically Templated Borates： [（C2H10N2）]2[B14O20（OH）6] and [C8H22N4][B5O6（OH）4]2

Two new nonmetal borates, [（C2H10N2）]2[B14O20（OH）6] 1 and [C8H22N4][B5O6（OH）4]2 2, have been synthesized under mild conditions and characterized by single-crystal X-ray diffraction, FTIR, elemental analysis and thermogravimetric analysis. Crystal data for compound 1： triclinic, space group P^-1, a = 8.4979（17）, b = 8.8498（18）, c = 10.065（2）A^°, α = 95.01（3）, β = 96.99（3）, γ = 116.82（3）°, V= 661.8（3）A^°^3, Z= 1, Mr = 697.63, Dc = 1.751 g/cm^3,μ = 0.163 mm^-1, F（000） = 356, the final R = 0.0372 and wR = 0.0968 （I 〉 2σ（I））; and those for compound 2： monoclinic, space group P21/c, a = 9.1867（18）, b= 14.118（3）, c = 10.334（2）A^°, β = 91.48（3）°, V = 1339.8（5）A^°^3, Z = 2, Mr = 610.46, Dc = 1.513 g/cm^3,μ = 0.135 mm^-1, F（000） = 632, the final R = 0.0350 and wR = 0.0912 （I 〉 2σ（I））. For both 1 and 2, the anionic units are interlinked via O-H…O hydrogen bonds to form a 3D supramolecular network, while the protonated cations are located in the free space of the inorganic borate framework and interact with the anions by electrostatic attraction and extensive N-H…O hydrogen bonds.     

Synthesis and Crystal Structure of Tetraaquacopper(II) Bis(5-fluorouracil-1-acetate) Tetrahydrate

1 INTRODUCTION 5-Fluorouracil (5-FU) is an antimetabolite with good antimicrobial and antitumor activities but has toxic side effects[1~4]. In order to improve the topical delivery of 5-FU and reduce the side effects, many derivatives of 5-FU have been synthesized, some of which are of improved activity. 5-Fluorou- racil-1-acetic acid is a member of the family[5~8], which belongs to the pyrimidine base and is a cyto-toxic analogue of the natural base thymine, and has proven useful in th…     

Synthesis and Structure of 〔Cu(μ-C_6H_5COO)_2(C_4H_8O)〕_2

1mTRODUCT1ONBinuclearcoppercomplexesareimportantnotonlyincoordinationchemistryandmagnetostructuralstudiesbutalsoinpracticalapplication.tliInanattempttoseekthedisPersionandemulationreagentsofCWM(themixtureofcoalandwater),thetitlecomP0undwassynthesizedbyanoxidativepreparationmethodt2i,whosesynthesisandstructurearedifferentfromthosedescribedbyWangetoft3i.Here,0nlythesynthesisandstructureofthetitlecomP0undarereportedandthestudiesofitsappli-cationareinprogress.2EXPERIMENTAL2.1Preparati0n…     

Inorganic-organic framework structures; M(II) ethylenediphosphonates (M = Co, Ni, Mn) and a Mn(II) ethylenediphosphonato-phenanthroline

The reaction of nickel, cobalt, and manganese with 1,2-ethylenediphosphonic acid or 1,2-ethylenediphosphonic acid and 1,10-phenanthroline under hydrothermal conditions resulted in the pillared layered structures Co2(H2O)2(O3PC2H4PO3) (I) and Ni2(H2O)2(O3PC2H4PO3) (II), which are isostructural to a zinc phase that has previously been characterized by X-ray powder methods. In addition, a 1D chain structure, Mn(HO3P(CH2)2PO3H)(H2O)2(C12H8N2) (III), and a pillared layered structure, Mn(HO3P(CH2)2PO3H) (IV), were obtained. The structures of these phases were solved by single-crystal X-ray diffraction methods. The crystallographic data are as follows: compound I P21/n (No. 14), a = 5.6500(11) A, b = 4.7800(10) A, c = 15.330(3) A, beta = 98.50(3) degrees, V = 409.47(14) A3, Z = 2; compound II P21/n (No. 14), a = 5.5807(11) A, b = 4.7205(9) A, c = 15.250(3) A, beta = 98.55(3) degrees, V = 397.28(13) A3, Z = 2; compound III C2/c (No. 15), a = 12.109(2) A, b = 15.328(3) A, c = 9.848(2) A, beta = 108.88(3) degrees, V = 1729.5(6) A3, Z = 4; compound IV P (No. 2), a = 5.498(5) A, b = 7.715(6) A, c = 8.093(7) A, alpha = 82.986(12) degrees, beta = 75.565(12) degrees, gamma = 80.582(12)degrees, V = 326.7(5) A3, Z = 2. Magnetic measurements show antiferromagnetic behavior below TN = 7 K for I and 13 K for II.     

Synthesis and Crystal Structure of Zinc Complex [Zn（bipy）3][Zn（SCN）4]

1 INTRODUCTION The design and synthesis of metal-organic frame-work structure have been studied widely during thepast decade not only because of their intriguing ar-chitectures but also their unexpected properties forpotential practical applications in a wide number offields, such as asymmetric catalysis, magnetism, pho-toluminescence and so on[1～3]. These novel struc-tures can be rapidly and efficiently synthesized fromsimple subunits, where the metal ions, bi- or multi-dentate organic l…     

Synthesis and Crystal Structure of 1-(o-methylphenyl)-2-(p-methoxyphenyl)-1,3,2-diazaphospholidin-4-thione-2-sulfide

11NTRODUCTIoNThederivativesofdiazaphospholidinoneorthecorrespondingthionesareknowntopossessinterestingbiologicalproperties,suchasherbicidalactivity"'2i.Inrecentyears,itwasreportedthatthel,4,2-diazaphospholindine-5-thione-2havegoodselectiveherbicidalactivity"'41.Tolookformoreeffectiveherbicideswithlowtoxicity,aseriesofnovel1-(o-methylphenyl)-2-(p-methoxyphenyl)-phospholidin-4-thione-sulfideshavebeensynthesizedandtheirmolecularstructuresstudied.PreliminarybioassaysshowthatthesecomPoundshaveg…     

Synthesis and Crystal Structure of （3R,4R）-5-（2,4-Dichlorobenzoyl）-4-（4-nitrophenyl）-6-（phenylamino）-3,4-dihydro-2H-thiopyran-3-carbonitrile

The title compound(C25H16Cl2N3O3S),as a thiopyran derivative,has been synthe-sized by the cyclization of an organic intermediate obtained from Baylis-Hillman adducts with a β-aroylthioamide using copper(I) salt as the catalyst.The crystal belongs to the monoclinic system,space group P21/c with a = 13.668(3),b = 8.4803(17) c = 21.999(4) ,β = 113.57(3)°,V = 2337.2(10) 3,Z = 4,Mr = 510.38,Dc = 1.451 g/cm3,μ = 0.401 mm-1,F(000) = 1048,the final R = 0.0487 and wR = 0.1079 for 3678 observed reflections with I > 2σ(I).     

Hydrothermal Synthesis and Crystal Structure of a Cadmium(Ⅱ) Polymer with One-dimensional Chain Structure: [Cd(MDPPz)(BDC)(H2O)]n

A metal-organic coordination compound formulated as [Cd(MDPPz)(BDC)(H2O)]n 1 (MDPPz = 11-methyldipyrido[3,2-a:2',3'-c]phenazine, BDC = 1,4-benzenedicarboxylate) has been hydrothermally synthesized and structurally characterized by elemental analysis, IR spectrum, fluorescence spectrum and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group C2/c, with a = 30.673(8), b = 9.623(3), c = 20.784(6) (A), β = 98.646(3)o, V = 6065(3) (A)3, C27H17CdN4O5, Mr = 589.85, Dc = 1.292 g/cm3, μ(MoKα) = 0.757 mm(1, F(000) = 2360, Z = 8, the final R = 0.0381 and wR = 0.0855 for 4191 observed reflections (I＞2σ(I)). 1 exhibits blue fluorescence property at room temperature.     

Synthesis,Spectroscopic Properties and Crystal Structure of (C4N2H12)2Zr(C2O4)4·H2O

The title compound (C4N2H12)2Zr(C2O4)4·H2O 1 was synthesized by the reaction of ZrOCl2·8H2O, H2C2O4·2H2O and piperazinium in aqueous solution. Single-crystal X-ray analysis has revealed that compound 1 (C16H26N4O17Zr, Mr = 637.63) crystallizes in the monoclinic system, space group P21/c with a = 9.0425(3), b = 13.3844(3), c = 19.1191(5)A, β = 98.365(1)o, V = 2289.34(11) A3, Z = 4, Dc = 1.850 g/cm3, F(000) = 1304, μ = 0.577 mm-1, the final R = 0.0240 and wR = 0.0628 for 4386 observed reflections with I > 2σ(I). X-ray crystal-structure analysis suggests that compound 1 consists of [Zr(C2O4)4]4- anion and two protonated piperazinium cations. The anions are linked through hydrogen bonds of piperazinium. FT-IR and Raman spectra clearly show the existence of oxalate groups in the crystal lattice.