A New 3D Supramolecular Network Formed by [Zn_3（2,6-Pyridinedicarboxylate）_3Cl_4]~（4-）and 4-Carboxypyridinium

A new compound [Zn3(C7NO4H3)3Cl4]·[C6NO2H6]4·4H2O (I) has been synthesized and structurally characterized by X-ray crystallography.It crystallizes in monoclinic,space group C2/c with a=16.9018(14),b=12.6902(10),c=25.1170(2),β=90.54°,V=5387.0(8)3,Z=4,Zn3C45H41Cl4N7O24,Mr=1401.76,Dc=1.728 g/cm3,F(000)=2840,μ(MoKa)=1.615 mm-1,the R= 0.0758 and wR=0.2060 for 3468 observed reflections (I 2σ(I)).Analysis of single-crystal X-ray diffraction data shows that compound I displays an interesting example of 3D supramolecular networks with perfect neutral and ionic hydrogen bonding array.     

Hydrothermal Synthesis and Crystal Structure of a Manganese(Ⅱ) Polymer with a Two-dimensional Network Structure:[Mn(pzdc)(phen)]_n·nH_2O

A metal-organic coordination compound formulated as [Mn(pzdc)(phen)]n·nH2O 1 (H2pzdc=pyrazine-2,3-dicarboxylic acid,phen=1,10-phenanthroline) has been hydrothermally synthesized and structurally characterized by elemental analysis,IR,TG and single-crystal X-ray diffraction.The title compound crystallizes in the monoclinic system,space group P21/n with a= 11.7689(18),b=11.7458(18),c=13.360(2),β=110.341(2)o,V=1731.7(5)3,C18H12MnN4O5,Mr=419.26,Dc=1.608 g/cm3,μ(MoKα)=0.803 mm-1,F(000)=852,Z=4,the final R=0.0323 and wR=0.0823 for 2831 observed reflections (I 2σ(I)).It exhibits an interesting two-dimen-sional network structure.     

3-乙氧基水杨醛缩N,N-双(3-胺基丙烷)-甲基氨Zn(Ⅱ)配合物的合成、晶体结构及荧光性质

The reaction of 3-ethoxysalicylaldehyde-N,N-bis (3-aminopropyl)methylamine with Zn (Ⅱ) acetate in CH3CH2OH followed by recrystallization in CH3CH2OH gave rise to colourless block crystals of 3-ethoxysalicylaldehyde-N,N-bis(3-aminopropyl)methylamine Zn(Ⅱ). The compound has been characterized by elemental analysis,IR spectrum, molar conductivity and X-ray diffraction structure determination single crystal. It crystallizes in monoclinic, space group P21/c with a=1.028 91(13) nm, b=1.400 35(12) nm, c=1.733 69(19) nm, V=2.476 6(5) nm3, Z=4, Mr=504.91, Dc= 1.354 g. cm-3, T=298(2) K, F(000)= 1 064,μ(Mo Kα)=0.102 7 cm-1, R =0.068 4 and wR =0.185 3for 2 940 observed reflections with I＞2σ(Ⅰ). The fluorescence properties of ligand and the complex also have been investigated. The results show that the fluorescence intensity of the Zn(Ⅱ) complex is very stronger than the ligand. In the crystal, the molecules form 1D chain structure by π-π stacking. CCDC: 675010.     

Synthesis,Structure, and Luminescent and Dielectric Properties of a Novel 1D Chain Zinc(Ⅱ) Complex {[Zn(DCImPyO)·(H_2O)_2·]·H_3O}_n

Under hydrothermal conditions, 4-(4,5-dicarboxy-1H-imidazol-2-yl)pyridine 1-oxide (H3DCImPyO) reacted with ZnCl2 to give the 1D chain complex {[Zn(DCImPyO)·(H2O)2·]·H3O}n (1). Single-crystal X-ray determination shows that complex 1 crystallizes in the monoclinic system, space group P2 1 /c with a=9.488(2), b=13.247(3), c=12.959(4) , β=126.716(19)°, Z=4, V=1305.6(6) 3 , C10H11N3O8Zn, D c=1.865 g/cm3 , M r=366.61, λ(MoKa)=0.71073 , μ=1.930 mm -1 , F(000)=744, R=0.0472 and wR=0.1487. Fluorescent analysis showed an intense emission band at 422 nm when the exciting radiation was set at 378 nm. Dielectric constant of complex 1 was measured at different frequencies with temperature variation.     

A novel heteropolymetalate containing Fe_4(OH)_4 segment: crystal structure of [Me_4N]_10[Fe_4(OH)_4(PW_10O_37)_2]·15H_2O

[Me4N]10[Fe4(OH)4(PW10O37)2] · 15H2O was synthesized by the reaction of FeCl3 ·6H2O, with △-Na8HPW9O34 and Me4NBr. Crystal data: M = 6225.75, space group P21/c with the monoclinic parameters: a = 1.3228(5), b = 3.5634(3), c = 1.5226(2) nm, β = 94.20(2)°, V = 7.1576nm3, 7 = 2,DC = 2.888 g/cm3, Mo Kαradiation (λ = 0.071069 nm), μ= 168.534 cm-1, F(000)=5576, final R = 0.0428 and Rw = 0.1204 for 7086 observed reflections with I > 2σ( I) . The structure of the title compound is the first structurally characterized heteropolymetalate with hydroxo-bridging metal aggregation Fe4OH4 encapsulated in the dimer of Keggin polyoxoanion.     

A Novel Two-dimensional Homochiral Zinc（II） Complex Constructed Based on In Situ Ligand Formation

A novel zinc(Ⅱ) complex, Zn(IBT) 2 (1, HIBT=5-(4-((1H-imidazol-1-yl)methyl)phenyl)-2H-tetrazole) has been synthesized with Zn(NO3)2·6H2O, 4-(imidazol-1-ylmethyl)benzonnitrile (IBN) and NaN 3 by the hydrothermal method, and characterized by elemental analysis, IR and single-crystal X-ray diffraction. Crystallographic data for 1:C22H18N12Zn, Mr=515.85, orthorhombic, Pbcn, a=16.0567(15), b=9.5316(9), c=14.6107(14) , V=2236.1(4)  3 , Z=4, D c=1.532 g/cm3 , μ=1.138 mm-1 , F(000)=1056, R=0.0350 and wR=0.0888 for 1438 observed reflections (I > 2σ(I)) and the goodness-of-fit S=1.002 on F2 . The crystal structural analysis revealed that complex 1 exhibits a rare two-dimensional homochiral wave-like layer structure. In addition, the photoluminescence of complex 1 was studied in the solid state at room temperature together with its theoretical analysis.     

Synthesis and Crystal Structure of a Zinc（Ⅱ）Complex with 2,2＇-Diphenic Acid and Benzimidazole Ligands

A new complex [Zn1.5(dpa)1.5(bim)]2n(dpa = 2,2-diphenic acid,bim = benzimida-zole)1 has been hydrothermally synthesized and structurally characterized by elemental analysis,IR,fluorescence spectrum and single-crystal X-ray diffraction.The complex crystallizes in monoclinic,space group C2/c with a = 18.773(8),b = 16.560(7),c = 16.417(9),β = 94.737(9)o,V = 5086(4)3,C56H36N4O12Zn3,Mr = 1153.00,Dc = 1.506 g/cm3,μ(MoKα)= 1.472 mm1,F(000)= 2344,Z = 4,the final R = 0.0573 and wR = 0.1164 for 2968 observed reflections(I > 2σ(I)).It exhibits a one-dimensional chain-like structure and shows luminescent property in the blue region.     

Syntheses and Crystal Structures of 1,5-Disubstituted 1,3,5-Hexahydro-triazine-2-（N-nitro）imines

The title compounds,C9H13ClN6O2S 1 and C15H17ClN6O2S 2,were synthesized and structurally characterized by elemental analysis,IR,1H NMR spectra and single-crystal X-ray diffraction.Compound 1 is in the monoclinic system,space group P21/c with a=13.7711(5),b=10.3883(4),c=9.7623(2),V=1344.47(8)3,Dc=1.506 g/cm3,C9H13ClN6O2S,Mr=304.76,F(000)=632,μ=0.448 mm-1,Z=4,S=1.084,R=0.0497 and wR=0.1328 for 2640 unique reflections(Rint=0.0787) with 2089 observed ones(I2σ(I)).Compound 2 belongs to the monoclinic system,space group P21/n with a=8.3828(5),b=14.5285(7),c=14.2456(4),V=1729.74(14)3,Dc=1.462 g/cm3,C15H17ClN6O2S,Mr=380.86,F(000)=792,μ=0.364 mm-1,Z=4,S=1.057,R=0.0598 and wR=0.1582 for 3384 unique reflections(Rint=0.0469) with 2833 observed ones(I2σ(I)).Compounds 1 and 2 are homologues and stabilized by intermolecular and intramolecular hydrogen bonds.Moreover,compound 2 containing C(2)-H(2)…π(thiazole) interaction is more stable than 1.     

一个新颖的二维锌配位聚合物[Zn(L)(1,4-BDC)]_n的合成、结构和表征(英文)

The title coordination polymer,[Zn (L) (1,4-BDC)]n (1) (L =2-(4-fluorophenyl)-1H-imidazo [4,5-f] [1,10] phenanthroline and 1,4-H2BDC=1,4-benzenedicarboxylic acid) has been synthesized by hydrothermal method and characterized by elemental analysis,IR and single-crystal X-ray diffraction. It crystallizes in triclinic,space group P1 with a=0.970 85(16) nm,b=1.076 98(18) nm,c=1.203 6(2) nm,α=63.894(2)°,β=69.051(2)°,γ=80.427(2)°,V= 1.055 4(3) nm3,Z=2,C27H15FN4O4Zn,Mr=543.80,Dc=1.711 g·cm-3,F(000)=552,μ(Mo Kα)=1.220 mm-1,R=0.037 2 and wR=0.084 4. The 1,4-BDC ligands linked the Zn(Ⅱ) atoms to form a two-dimensional layer structure. The π-π stacking interactions between L ligands extended the adjacent layers into a three-dimensional supramolecular network. Finally,the N-H…O hydrogen bonds further stabilizes the structure of 1.     

一个新颖的(5,6)-连接三维超分子网络拓扑结构(英文)

A new complex,[Co(HL)2(H2O)4]·H2O(1)(H2L =5-carboxy-1-carboxymethyl-2-oxidopyridinium),was synthesized and characterized by X-ray single-crystal diffraction,elemental analysis,and IR spectra.The crystal is monoclinic,space group P21/c with a=0.512 69(2) nm,b=2.275 31(1) nm,c=1.003 95(6) nm,β=98.015(3)°,V= 1.159 7(1) nm3,Z=2,Mr=541.29,F(000)=558,Dc=1.550 g·cm-3,μ=0.816 mm-1,the final R=0.044 5 and wR=0.142 1 for 2 015 observed reflections(I2σ(I)).Complex 1 can be considered constructed from 2D layers,which consist of left-and right-handed helical chains and further linked into a 3D supramolecular architecture by hydrogen bonds.Topology analysis reveals that complex 1 shows an unprecedented 3D binodal(5,6)-connected topology.     

Two 3-D Neutral Zn(Ⅱ)-MOFs Generated from the Asymmetric Schiff-base Ligand

Two new Zn(Ⅱ)-MOFs were synthesized based on an asymmetric Schiff-base ligand LH, which is obtained by the condensation of 5-formyl-8-hydroxyquinoline and 3-pyridinecarboxylic acid hydrazide. In different mixed solvents, we get two new isomorphism compounds, [Zn(L)2]·C4H8O2·2MeOH(1) and [Zn(L)2]·CH2Cl2·2MeOH(2). Compounds 1 and 2 have been characterized by single-crystal X-ray diffraction, elemental analysis and IR. Compound 1 crystallizes in monoclinic, space group P21/c, with a = 13.856(4), b = 14.156(4), c = 9.620(3) , β = 110.167(5)°, V = 1771.3(9) 3, Dc = 1.500 g/cm3, C38H38N8O8 Zn, Mr = 800.13, F(000) = 832, μ(MoKα) = 0.761 mm-1, Z = 2, the final R = 0.0596 and wR = 0.1221 for 2112 observed reflections(I 2σ(I)). Compound 2 belongs to monoclinic, space group P21/c, with a = 13.575(3), b = 14.130(3), c = 9.485(2) , β = 107.908(3)°, V = 1731.2(6) 3, Dc = 1.529 g/cm3, C35H32Cl2N8O6 Zn, Mr = 796.96, F(000) = 820, μ(MoKα) = 0.926 mm-1, Z = 2, the final R = 0.0527 and wR = 0.1395 for 2501 observed reflections(I 2σ(I)). The Zn(Ⅱ) centers in both 1 and 2 display a distorted octahedral coordination geometry. The octahedral Zn(Ⅱ) nodes and L linkages build up 2-D nets consisting of parallelogram-like grids in the ab plane. The neighboring nets stack through hydrogen bonds to generate 3-D rhombic channels. In 1, the 1,4-dioxane and MeOH guests alternatively arrange in the channels and effectively take up the free space; while in 2, the CH2Cl2 guests are arranged in the channels. In addition, the encapsulated MeOH molecules are bonded to the framework by hydrogen bonds.     

Hydrothermal Synthesis and Crystal Structure of a 2D Zinc（Ⅱ） Coordination Polymer with 5-Hydroxynicotinic Acid

The title compound,[Zn(5-hydroxynicotinate) 2 2H 2 O] n,has been synthesized by reacting zinc sulfate vitriol with 5-hydroxynicotinic acid under hydrothermal conditions,and its structure was determined by X-ray crystallography with the following data:monoclinic,space group C2/c,C 12 H 12 N 2 O 8 Zn,M r=377.61,a=10.223(3),b=10.319(3),c=13.613(4),β=105.922(6)°,Z=4,V=1380.9(8)3,F(000)=768,D c=1.816 g/cm 3,μ(MoKα)=1.826 mm-1,the final R=0.0401 and wR=0.1380 for 1157 observed reflections (I > 2σ(I)).In the structure of the title compound,the Zn II ion located in an inversion center lies in a distorted tetrahedral environment at a N 2 O 2 coordination mode,and the 5-hydroxynicotinic acid ligand links symmetry-related Zn II ions at a μ 2-N,O bridging way forming a two-dimensional covalent structure.In the crystal,solvent water molecules form intermolecular O-H O hydrogen bonds and pyridine rings of adjacent layers form π-π stacking (3.346),which connect adjacent two-dimensional sheets into a three-dimensional supramolecular network.     

Crystal Structure and Conformation of [1-(β-D-lyxofuranosyl)uracil]-2′-spiro-5″-[4″-(S)-(diethoxyphosphinyl)-2″-oxazoline]

The title compound, C15H22N3O9P·2H2O, Mr=455.36, crystallizes in orthorhombic, space group P212121, with a =9.193(2), b =14.681(3), c =15.201(3)A, V =2501(1)A3, Z =4, Dx=1.474g/cm3, λ(MoKα)=0.71073A, μ=0.1894mm-1, T=299±1K, F(000)=960, R=0.061 and Rw=0.068 for 1899 observed reflections with I≥3σ(I). The analysis results indicate that the title compound is of lyxo-configuration and the configuration at C4″ is S. In the crystal state the molecule has anti conformation about glycosidic bond with the torsion angle-151.7°, the sugar ring is puckered with C3′-endo-C2′-exo, and the conformation of the C4′-C5′ bond is-sc.     

三核镍配合物Ni_3(C_(14)H_8N_3O_5)_2(C_5H_5N)_4的合成、晶体结构和抗癌活性(英文)

The title complex Ni3(C14H8N3O5)2(C5H5N)4 has been synthesized by the reaction of 2-hydroxy-N′-(4- nitrobenzoyl)benzohydraizide with nickel acetate in pyridine solution. Its molecular structure was characterized by elemental analysis, IR spectra and X-ray crystal structure determination. Crystal data for this compound: Mono- clinic, space group P21/c, Mr=1 089.00, a=0.249 27(5) nm, b=0.161 40(3) nm, c=0.121 81(2) nm, β=94.59(3)°, V= 4.885 2(17) nm3, Z=4, Dc=1.481 Mg·m-3, F(000)=2 232, R1=0.049 7, wR2=0.106 8 (observed reflections with I2σ(I)) and R1=0.105 1, wR2=0.119 4 (all reflections), GOF=1.021. The complex was evaluated for their antitumor activi- ties against two kinds of cell lines (K562 and BGC) by MTT method. A preliminary bioactivity study indicates that the complex shows distinct antitumor activity.     

Two Isostructural 2-D Metal(Ⅱ)-organic Coordination Polymers from 4,4'-Bipyridyl and (E)-2,6-Dimethyl-4-styrylpyridine-3,5-dicarboxylic Acid

(E)-2,6-Dimethyl-4-styrylpyridine-3,5-dicarboxylic acid (H2mspda) is firstly employed in coordination chemistry.Two isostructural two-dimensional (2-D) 4-connected metal-organic coordination polymers with a general formula of {M2[(mspda)2(bpy)(H2O)2]}n (M=Zn(1) and Co(2)) are assembled from H2mspda,4,4'-bipyridyl (bpy),zinc and cobalt ions under hydrothermal conditions,and characterized by single-crystal X-ray diffraction analyses.Complex 1 crystallizes in monoclinic,space group P21/n with a=14.551(4),b=10.941(3),c=14.945(4),β=98.817(4)o,V=2351.3(1)3,Dc=1.511 g/cm3,μ(MoKα)=1.090 mm-1,F(000)=1104,Z=4,the final R=0.0335 and wR=0.0485 for 3296 observed reflections (I 2σ(I)).In compound 1,mspda2-spacers are only arrayed in a head-to-tail fashion which corresponds to a 2-D coordination polymer.Solid-state H2mspda and complex 1 have expected photoluminescence (λem=475～496 nm) at room temperature.     

Synthesis and Crystal Structure of Bis(isonitrosoethylacetoacetate- N- benzylimino) palladium (Ⅱ)

The title complex Pd(C13H15N2O3)2(C13H15N2O3))- is the anion of isonitrosoethylacetoacetate-N-benzylimine) crystallizes in the monoclinic system, space group P21/c with a= 8. 197(2), b= 14. 524(3), c= 10. 835(2) A , β= 101.77(3)°, V= 1262. 8(5) A3, Dc=1. 580 g/cm3, F(000)=616, Mr= 600. 94, μ(MoKα) =0. 784mm-1, Z=2 and final R=0. 0410 and wR=0. 0962 for 1855 observed reflections [I≥2σ(I)]. The geometry around the palladium atom is a distorted trans PdN4 square plane, the Schiff base ligand C6H5CH2-IEAI- being coordinated through its oximo-nitrogen atom and imino-nitrogen atom.     

Hydrothermal Synthesis and Crystal Structure of a Zinc(Ⅱ) Polymer with a Two-dimensional Layer Structure: [Zn(pzdc)(phen)] n·nH_2O

A metal-organic coordination compound formulated as [Zn(pzdc)(phen)] n·nH_2O 1 (H_2pzdc=pyrazine-2,3-dicarboxylic acid,phen=1,10-phenanthroline) has been hydrothermally synthesized and structurally characterized by elemental analysis,IR,fluorescence spectrum and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system,space group P2_(1/n) with α=11.607(2),b=11.719(2),c=13.140(3)(A),β=110.707(3)°,V=1671.9(6)(A)~3,C_(18)H_(12)ZnN_4O_5,Mr=429.69,D_c=1.707 g/cm~3,μ(MoKα)=1.511 mm~(-1),F(000)=872,Z=4,the final R=0.0356 and wR=0.0853 for 2713 observed reflections (Ⅰ> 2σ(Ⅰ). It exhibits an interesting two-dimensional layer structure and shows yellow photoluminescent property at room temperature.     

Syntheses and Crystal Structures of Two Tin(Ⅳ) Complexes with Aminosilane Bearing Ligand

Aminosilane bearing bulky substituents on nitrogen: LH2(L=Me2Si(NDipp-)2 , Dipp=2,6-diisopropylphenyl) was reacted with BuLi in toluene. The resulting bulky chelating dianion Me2Si(NDipp-)2 was used to synthesize the unusual spirocyclic heterotriatomic complex [Me2Si(NDipp)2]2Sn (1) by its reaction with SnCl4 and the bulky heterotriatomic complex Me2Si(NDipp)2SnPh2 (2) with Ph2SnCl2.1 belongs to the monoclinic system, space group P21/n with a=13.193(2), b=20.663(3), c=20.403(3), β=99.954(2)o, V=5478.3(15)3 , C55H85.5N4Si2Sn, Mr=977.64, Z=4, Dc=1.185Mg/m3 , μ(MoKα)=0.547mm-1 , F(000)=2086, S=1.000, the final R=0.0614 and wR=0.1322 for 14446 observed reflections (I2σ(I)) and R=0.0797 and wR=0.1456 for all data. 2 belongs to the triclinic system, space group Pī with a=10.36(15), b=13.204(7), c=14.363(7), α=90.214(10), β=106.182(7), γ=109.854(8)o, V=1764.4(15)3 , C38H50N2SiSn, Mr=681.58, Z=2, Dc=1.283 Mg/m3 , μ(MoKα)=0.785 mm-1 , F(000)=712, S=1.002, the final R=0.0498 and wR=0.0955 for 7533 observed reflections (I2σ(I)) and R=0.0676 and wR=0.1018 for all data. In the structure of 1, the tin atom is located in the spirocyclic center of the two fused four-membered SnN 2 Si rings. The two complexes were characterized by 1H NMR, elemental analysis, and single-crystal X-ray structural analysis.     

Synthesis and Crystal Structure of N-[2-（4-Chlorophenyl）-1-（1-methylcarbamoyl-2-phenyl-ethylcarbamoyl）-3-phenyl-cyclopropyl]-benzamide

N-[2-(4-chlorophenyl)-1-(1-methylcarbamoyl-2-phenyl-ethylcarbamoyl)-3-phenyl-cyclopropyl]benzamide,C33H30ClN3O3,has been synthesized and characterized by IR,1H NMR,13C NMR and single-crystal X-ray diffraction.The crystal is of triclinic,space group P1 with a = 11.646(2),b = 13.795(3),c = 14.559(3),α = 76.422(4),β = 78.028(4),γ = 74.500(4)°,V = 2164.6(7)3,Z = 3,Mr = 552.05,Dc = 1.270 g/cm3,λ = 0.71073 ,μ(MoKα)= 0.171 mm–1,F(000)= 870,the final R = 0.0469 and wR = 0.0805 for 5554 observed reflections with I > 2σ(I).The N–H and oxygen atoms are involved in one-dimensional intermolecular hydrogen bonds,which further stabilize the structure.     

Solvothermal Synthesis and Crystal Structure of a Zn（II） Microporous Metal-organic Framework

A novel three-dimensional Zn(Ⅱ) coordination polymer, Zn3(C2H2N3)4(SiF6), has been synthesized under solvothermal conditions using 1H-1,2,4-triazole-3-carboxylic acid and zinc fluoride as the starting materials. The complex has been characterized by elemental analysis, IR, TG analysis and single-crystal X-ray diffraction analysis. The complex crystallizes in the tetragonal I4/mmm space group with a=11.592(0), c=7.526(1), V=1011.3(2)3 , Z=2, Mr=610.46, Dc=2.005 g/cm3 and F(000)=596. The final R=0.0312 and wR=0.067 for 319 observed reflections with I>2σ(I). In the title complex, the Zn centers are interconnected by μ 3 -bridging triazole ligands to form a microporous three-dimensional metal-organic framework.