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.     

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）A, β = 109.187（2）°, V = 1482.6（2）A^3, Z = 1, C52H52N8O23Zn4, Mr = 1418.58, Dc = 1.589 g/cm^3, 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,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.     

Crystal Structure and Antitumor Activity of Tri[2-[N-（4′-methyl-benzylsulfonyl）amino]ethyl]-amine

The crystal structure of the title compound (C27H38N4O7S3, Mr = 626.79) has been determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group Pīwith a = 9.411(1), b = 11.645(2), c = 14.672(2) (A。), α = 91.80(1), β = 95.36(1), γ =104.56(1)o, V = 1547.0 (A。)3, Z = 2, Dc = 1.346 g/cm3, λ = 0.71073 (A。), μ(MoKα) = 0.289 mm－1 and F(000) = 664. The structure was refined to R = 0.0406 and wR = 0.1177 for 4103 observed reflections with I > 2σ(I). X-ray diffraction analysis reveals that the title compound is a practically distorted tetrahedron and each molecule contains one lattice H2O by hydrogen bond. The antitumor activity of the title compound against HL-60 human leukemia cells has also been studied by MTT method.     

Synthesis,Crystal Structure and Anti-integrase Activity of 25,27-Bis[(Z)-4-(p-methoxyphenyl)-4-hydroxybut-3-en-2-one-1-methyl]-26,28-dihydroxycalix [4] arene

The title compound(C50H44O10) was synthesized and structurally determined by single-crystal X-ray diffraction method. It crystallizes in monoclinic, space group P21/c with a = 16.713(4), b = 13.189(3), c = 19.434(5) , β = 104.411(4)°, Mr = 804.85, Dc = 1.288 g/cm3, V = 4149.2(17) 3, Z = 4, F(000) = 1696, μ(MoKa) = 0.089 mm-1, T = 296(2) K, 7279 independent reflections with 3172 observed ones(I 2σ(I)), R = 0.0520 and wR = 0.1203 with GOF = 0.928(R = 0.1464 and wR = 0.1657 for all data). The calixarene moiety maintains the symmetric cone conformation through intramolecular O–H···O hydrogen bonds. Preliminary bioassays indicated that the title compound has a potent inhibitory activity against the strand transfer process of HIV-1 integrase.     

Crystal Structure and Biological Activities of N-(5-(4-Chloro-2-(trifluoromethyl)phenyl)furan-2- carbonyl)-N'-(4,6-dimethylpyrimidin-2-yl)thiourea

The new title compound N-(5-(4-chloro-2-(trifluoromethyl)phenyl)furan-2-carbon-yl)- N?-(4,6-dimethylpyrimidin-2-yl)thiourea (C19H14ClF3N4O2S) has been synthesized, and its crystal structure and biological behaviors were studied. The title compound crystallizes in the monoclinic system, space group P21/c with a = 7.932(5), b = 33.46(2), c = 7.556(5) , β = 98.058(9)°, V = 1986(2) 3, Mr = 454.85, Z = 4, Dc = 1.521 g/cm3, μ = 0.349 mm–1 and F(000) = 928. The structure was solved by direct methods and refined to R = 0.0724 and wR = 0.1429 for 3494 observed reflections (I > 2σ(I)). Intermolecular hydrogen bonds along the b axis together with the continuous π-π interactions construct the three-dimensional architecture of the title compound. The preliminary biological tests show definite herbicidal activity for the title compound.     

A Novel 3D Supramolecular Framework of Poly[(5-(oxidediphenylphosphino)isophthalate)zinc(Ⅱ)]: Syntheses and Structure

A novel metal-organic framework, namely [Zn(C20H13O5P)]n(1), has been hydrothermally synthesized through the reaction of 5-(oxidediphenylphosphino)isophthalic acid(H2L) with Zn(Ⅱ) salt. The title compound crystallizes in monoclinic, space group P21/c with a = 11.0966(10), b = 14.5651(14), c = 14.7311(15), β = 130.022(6)o, C20H13O5 PZn, Mr = 429.64, V = 1823.3(3) 3, Dc = 1.565 g/cm3, F(000) = 872, μ = 1.463 mm-1, S = 1.054 and Z = 4. The final R = 0.0270 and wR = 0.0739 for 2769 observed reflections with I 2σ(I). In the title complex, the Zn2(CO2)2 binuclear clusters are linked by L2- ligands to result in a pillared layer structure in the bc plane, which is a(4,4)-net composed of helical chains with opposite chirality by sharing Zn2(CO2)2 units. Adjacent layers are further associated together through Zn–O bonds involving the metal center and the oxygen atom of P=O group to achieve a 3D architecture, in which one-dimensional quadrangled channel displays the interweaving of two pairs of coaxial double-helical chains with opposite chirality. The luminescence property and thermogravimetric analysis of the title complex were investigated.     

Synthesis,Structure and Luminescent Properties of [Zn(btzb)2Cl2]·2H2O[btzb=1,2-Bis(5-tetrazolyl)benzene]

The title compound[Zn(btzb)2Cl2]·2H2O(1·2H2O,btzb=1,2-bis(5-tetrazolyl)benzene)was synthesized in situ by the[2 3] cycloaddition reaction of phthalonitrile with NaN3 in water in the presence of ZnCl2 under refluxing conditions.1·2H2O crystallizes in the monoclinic system,space group P21/c with a=9.0119(18),b=7.5566(15),c=18.076(5)(A),β=114.67(2)°,V=1118.6(4)(A)3,Z=2,Dc=1.784 g/cm3 T=223(2)K,C16H16N16O2Cl2Zn,Mr=600.74,F(000)=608,μ(MoKα)=1.393 mm-1,S=1.081,R=0.0306 and wR=0.0669 for 1896 observed reflections with Ⅰ ＞2σ(Ⅰ).The Zn2 ion of 1 is coordinated by four N atoms from two btzb ligands and two Cl atoms,forming a distorted octahedral coordination geometry.A number of intermolecular hydrogen bonding interactions between molecules 1 and/or the solvated water molecules result in a 3D hydrogen-bonded structure.The luminescent property of 1·2H2O was also investigated.     

Synthesis and Crystal Structure of Bis（p—aminotoluene）—bis（dimethylglyoximato） Cobalt（Ⅲ） Perchlorate

The title compound (C22H32.5ClCoN6O8.25,Mr=607.42)crystallizes in the orthorhombic system,space group c222 1 with a=11.320(2),b=20.933(4),c=23.936(5)A,V=5672(2)A^3,Dc=1.423g/cm^3,Z=8,μ(MoKα）=0.754mm^-1,F(000)=2532,R=0.0512 and wR=0.1190,There are eight complex molecules [Co(C4H6N2O2)(C4H8N2O2)(C7H9N)2]ClO4.0.25H2O of C2 crystallographic symmetry in a unit cell,including two crystallographically independent molecules,in which different orientations of the MePhNH2 groups are found.Two MephNH2 groups are in trans position for molecule A,and cis for B.The central metal atom is in a distroted octahedral environment.The hydrogen bonds of O-H(oxime)…O and N-H(p-aminotoluene group)…O construct an one-dimensional chain along the c axis in the title compound.     

Synthesis and Crystal Structure of 4,4＂-Diamino-N,N＇-diethyl Bisbenzenesulfamide

A new compound of 4,4'-diamino-N,N'-diethyl bisbenzenesulfamide (C18H26N4O4S2,Fw = 426.55) has been synthesized and its structure was determined by X-ray crystallography method. The crystal belongs to the monoclinic system, space group P21/c with a = 10.0623(9), b =13.6759(13), c =15.5309(14) (A),β = 100.482(2)°, V= 2101.6(3)(A)3, Dc = 1.348 g/cm3, F(000) = 904,μ = 0.285 mm-1, Z = 4, the final R = 0.0512 and wR = 0.1363 for 3485 observed reflections with I ＞2σ(Ⅰ). The structure of the title compound is pseudo secondary axisymmetric, and the two sulfamide-groups show distorted tetrahedral configurations.     

Hydrothermal Synthesis and Crystal Structure of a Copper Complex

The title compound [Cu(IB)2]n·n(H2O) 1 was synthesized via the hydrothermal reaction of CuSO4·5H2O and NaOH with 4-(1H-Imidazol-1-yl)benzoic acid(HIB),and character-rized by elemental analysis and infrared spectra.The crystal of 1 crystallizes in monoclinic,space group C2/c with a = 14.349(7),b = 5.977(3),c = 21.368(9) ,β = 104.956(9)o,V = 1770.5(2)3,Z = 4,C20H16CuN4O5,Mr = 455.92,Dc = 1.710 g/cm3,F(000) = 932 and μ(MoKα) = 1.279 mm-1.The final R = 0.0337 and wR = 0.0888 for 1972 observed reflections with Ⅰ 2σ(Ⅰ) and R = 0.0369 and wR = 0.0926 for all data.X-ray diffraction reveals that the IB ligand links the Cu(Ⅱ) atoms into a double stranded chain.The extensive supramolecular interactions lead to the formation of an infinite 2D structure.     

A Three-dimensional Neodymium（Ⅲ）- potassium（Ⅰ） Coordination Polymer

The title compound [NdK（btec）（H2O）2]n 1 was synthesized via the hydrothermal reaction of Zn（OAc）E·H2O, Nd（NO3）3 and KOH with 1,2,4,5-benzenetetra-carboxylic acid （H4btec）, and characterized by elemental analysis and infrared spectra. The crystal of 1 crystallizes in monoclinic, space group P21/c with a = 8.9023（3）, b = 7.8954（1）, c = 17.6249（5）A,β= 91.857（1）°, V= 1238.16（6）A^3, Z = 4, C10H6KNdO10, Mr= 469.49, Dc = 2.519 g/cm^3, F（000） = 900 andμ（MoKa） = 4.585 mm^-1. The final R = 0.0404 and wR = 0.0832 for 2197 observed reflections with I 〉 2σ（I） and R = 0.0431 and wR = 0.0854 for all data. X-ray diffraction reveals that the btec ligand serves as a μ16-bridging ligand to link the Nd（Ⅲ） and K（Ⅰ） atoms into a three-dimensional coordination polymer. Photoluminescent investigation shows that the title compound displays strong emission in the blue region, which may be attributed to an intraligand emission state.     

Synthesis and Crystal Structure of N-[(3aR,4R,4aR,5aS,6S,6aS)-1,3-Dioxooctahydro-4,6-ethenocyclopropa[f]isoindol-2(1H)yl]-4-(trifiuoromethyl)phenylmethanimine Monohydrate

The crystal structure of the title compound (C19H17F3N2O4,Mr=394.35) was determined by single-crystal X-ray diffraction.The crystal belongs to monoclinic,space group C2/c with a=28.383(6),b=10.355(2),c=12.799(3)(A),β=111.74(3)°,V=3493.8(12)(A)3,Z=8,De=1.499 g/cm3,λ(MoKα)=0.71073,F(000)=1632,μ= 0.127 mm-1,R=0.0412 and wR=0.1019.In the title compound,there exist three intennolecular hydrogen interactions (O(4)...O(1),O(4)...O(3) and O(4)...N(1)) between water.The neighboring molecules are linked to each other generating a two-dimensional network structure via the three intermolecular hydrogen bonds and π-π interactions shaped by phen-phen with centroid distance of 4.049 (A).     

Synthesis and Crystal Structure of（2E,6E）-2,6-bis（2,3-dimethoxybenzylidene）cyclohexanone

The new title compound (2E,6E)-2,6-bis(2,3-dimethoxybenzylidene)cyclohexanone (C 24 H 26 O 5,M r=394.45) has been synthesized,and its crystal structure was studied.The title compound crystallizes in the orthorhombic system,space group Pca2 1 with a=17.536(2),b=14.8515(16),c=8.0512(9),V=2096.8(4) 3,Z=4,D c=1.250 g/cm 3,λ=0.71073,μ=0.087 mm-1 and F(000)=840.The structure was solved by direct methods and refined to R=0.0533 and wR=0.1248 from 2727 observed reflections (I > 2σ(Ⅰ)).The title molecules are connected through hydrogen bonds to generate a 3-D supramolecule.The preliminary biological tests showed definitely biological activity for the title compound.     

Hydrothermal Synthesis and Crystal Structure of a Manganese Complex

The title compound [Mn(Phen)(p-MBA)2]n(1) was synthesized via the hydro-thermal reaction of KMnO4 and NaOH with phen and p-methybenzoic acid(p-MBA) in water.The title compound was characterized by elemental analysis and infrared spectra.The crystal of 1 crystallizes in orthorhombic,space group Pbcn with a = 24.132(1),b = 10.404(0),c = 9.386(0) ,V = 2356.65(13) 3,Z = 4,C28H22MnN2O4,Mr = 505.42,Dc = 1.424 g/cm3,F(000) = 1044 and μ(MoKα) = 0.598 mm-1.The final R = 0.0781 and wR = 0.1363 for 1972 observed reflections with Ⅰ 2σ(Ⅰ) and R = 0.0897 and wR = 0.1420 for all data.X-ray diffraction reveals that the Phen and p-methy benzoic acid ligand link the Mn atoms into a single one-dimensional coordination polymer,and extensive intermolecular π-π interactions lead these 1D chains to form a two-dimensional supramolecular architecture.     

Synthesis and Crystal Structure of a Nitronyl Nitroxide Complex {[Zn(NIT4Py)(fum)(H2O)2]·H2}n

The title compound {[Zn(NIT4Py)(fum)(H2O)2]·H2O}n, where N1T4Py=2-(4'-pyridinyl)-4,4,5,5-tetra-methylimidazoline-l-oxyl-3-oxide and rum=fumarate, has been prepared and structurally characterized by X-ray diffraction. It crystallizes in triclinic, space group P1 with a =6.9533(9), b=9.805(1), c=15.248(2)A, a=94.608(2), β=92.328(2),γ=105.840(2)°,C16H24N3O9Zn, Mr=467.75, V=994.8(2) A3, Z=2, Dc=1.562 g/cm3,μ(MoKa)=1.289 mm-1,F(000)=486, the final R=0.0243 and wR=0.0622 for 3505 independent reflections with Rint=0.0125. The Zn(Ⅱ) adopts a distorted five-coordinate triangle bipyramidal geometry. The basic framework structure of the complex is a 1-D chain. The intrachain hydrogen bonds are helpful to stabilize the 1-D chain structure. Furthermore, the chains are connected by O-H…O hydrogen bonds to give a 2-D double-layer network.     

Synthesis, Structure and Geometrical Calculation of a Novel Co-crystal of {[4-Bromo-2-(benzimidazol-2-yl)phenolato][2- (1-butylbenzimidazol-2-yl)phenolato]zinc(Ⅱ)] and Bis[μ-2- (1- butylbenzimidazol-2-yl)phenolato]- 1κN3: 2κO; 1κO:2κN3-bis{[2-(1-butylbenzimidazol-2-yl)phenolato-κ2N3,O]zinc(Ⅱ)}

The title compound has been synthesized and characterized crystallographically. It is a co-crystal consisting of two different neutral zinc(Ⅱ) complexes with Hbpbm (Hbpbm = 4-bromo-2-(benzimidazol-2-yl)phenol) and Hnpbm (Hnpbm = 2-(1-butylbenzimidazol-2-yl)phenol).One is a monomeric mixed-ligand complex of [Zn(bpbm)(npbm)] 1 and the other a dimer of[Zn2(npbm)4] 2 with their ratio of 2:1. Thus the overall formula for the title compound is 21·2.Adjacent 1 and 2 are connected to each other by intermolecular hydrogen bonding interactions in the lattice. The crystal data: monoclinic, space group P21/c, a= 15.0141(12), b = 20.9941(17), c =18.4686(15) (A), β = 97.445(2)°, V= 5772.4(8) (A)3, Mr= 2429.68, Z = 2, Dc = 1.398 g/cm3,μ = 1.579mm-1, F(000) = 2504, R = 0.0637 and wR = 0.1771 for 6464 observed reflections (I＞ 2σ(Ⅰ)). The geometrical structure for 1 has also been theoretically optimized and compared with the experimental one.     

Synthesis,Structure and Luminescent Property of a New Zn(Ⅱ) Coordination Polymer Based on 1,3,5-Benzenetricarboxylate and 4,4'-Bipyridine Ligands

A new Zn(II) coordination polymer [Zn3(BTC)2(4,4'-bpy)(CO)2]n(1, H3 BTC =1,3,5-benzenetricarboxylic acid, 4,4'-bpy = 4,4'-bipyridine) has been prepared through urothermal reaction of zinc nitrate hexahydrate with 1,3,5-benzenetricarboxylic acid and 4,4'-bipyridine, and characterized by elemental analysis, IR spectroscopy, TGA and powder XRD, and its crystal structure was determined by single-crystal X-ray diffraction analysis. The title compound crystallizes in the monoclinic system, space group C2/c, with a = 10.262(3), b = 18.838(5), c =15.083(4) A, β = 99.203(4)o, V = 2878.3(14) A3, C30H14Zn3N2O14, Mr = 822.54, Z = 4, Dc = 1.898g/cm3, μ = 2.561 mm-1, F(000) = 1640, R = 0.0363 and w R = 0.0932 for 2828 observed reflections(I 2σ(I)). X-ray analysis shows that the asymmetric unit of the title compound contains two crystallographically unique Zn(II) atoms which are connected by BTC3- ligands and 4,4'-bpy coligands to form a 3D framework with 1D channels. The solid luminescence of ligand and the title complex was also studied at room temperature.     

Synthesis and Crystal Structure of 4,4′-Diamino-N,N′-diethyl Bisbenzenesulfamide

A new compound of 4,4′-diamino-N,N′-diethyl bisbenzenesulfamide (C18H26N4O4S2, Fw = 426.55) has been synthesized and its structure was determined by X-ray crystallography method. The crystal belongs to the monoclinic system, space group P21/c with a = 10.0623(9), b = 13.6759(13), c =15.5309(14) , β = 100.482(2)o, V = 2101.6(3) 3, Dc = 1.348 g/cm3, F(000) = 904, μ = 0.285 mm–1, Z = 4, the final R = 0.0512 and wR = 0.1363 for 3485 observed reflections with I > 2σ(I). The structure of the title compound is pseudo secondary axisymmetric, and the two sulfamide-groups show distorted tetrahedral configurations.     

Synthesis,Crystal Structure and Antitumor Activity of 4-(tert-butyl)-5-(1H-1,2,4-triazol-1-yl)-N-(2-hydroxy-3,5-diiodinebenzyl)-thiazol-2-amine

The title compound, 4-(tert-butyl)-5-(1H-1,2,4-triazol-1-yl)-N-(2-hydroxy-3,5-diiodinebenzyl)thiazol-2-amine, was synthesized via the reduction of 4-(tert-butyl)-5-(1H-1,2,4-triazol-1-yl)-N-benzylidene-thiazol-2-amine with Na BH4, and its crystal structure was determined by single-crystal X-ray diffraction. The compound crystallizes in monoclinic system, space group P21/c with a = 7.91944(19), b = 10.5250(3), c = 24.4985(6) , Z = 4, V = 2041.66(9) 3, Mr = 599.22, Dc = 1.949 Mg/m3, S = 1.120, μ = 3.203 mm-1, F(000) = 1152, the final R = 0.0283 and wR = 0.0592 for 3490 observed reflections(Ⅰ 2σ(Ⅰ)). X-ray analysis displays that the crystal water takes part in three intermolecular hydrogen bonds of O(2)–H(2A)···O(1), O(2)–H(2B)···N(1) and N(5)–H(5)···O(2), and an octatomic ring is formed via intramolecular hydrogen bond of O(1)–H(1A)···N(4). Furthermore, the Ⅰ···Ⅰ contacts are involved in stabilizing the overall three-dimensional network structure. The preliminary biological test shows the title compound has good antitumor activity with the IC50 value of 26 μM against the Hela cell line.