A Zinc TTR Complex with a Novel 2-D Structure （TTR = 3-Amino-1H-1,2,4-triazole）

The solvothermal reaction of 3-amino-1H-1,2,4-triazole (ttr) with Zn(ClO4)2·6H2O and NaCl in a 1:1:1 molar ratio gave a new complex [Zn(ttr)Cl]n with a 3-connected (4.82) 2-D struc- ture. The layers stack in the -ABAB- way along the c axis with abundant hydrogen bonding interac- tions to form the crystal structure. The complex [Zn(ttr)Cl]n crystallizes in the orthorhombic space group Pbca with a = 9.369(1), b = 10.049(1), c = 11.905(1) , V = 1120.9(3) 3, Z = 8.00, C2N4H3ZnCl, Mr = 183.90, Dc = 2.180 g/cm3, μ = 4.740 mm-1, F(000) = 720, S = 1.059 and T = 293(2) K. The final R = 0.0662 and wR = 0.2457 for 956 observed reflections with I > 2σ(I), and R = 0.0689 and wR = 0.2504 for all data.     

Synthesis and Structure of 1.5Zn(phen)_3·L·3NO_3 Supramolecule(phen=o-Phenanthroline,L=4-Aminoacetophenone Thiosemicarbazone)

A supramolecular framework,1.5Zn(phen)3·L·3NO3(C63H48Zn1.5N16O9S),has been synthesized.The ligand L was synthesized by the condensation of p-aminoacetophenone with thiosemicarbazide.The crystal belongs to the monoclinic system,space group C2/c,with a = 31.005(2),b = 15.114(2),c = 24.887(3) ,β = 94.260(2)o,Z = 8,V = 11630(2) 3,Dc = 1.489 g/cm3,Mr = 1303.29,λ(MoKα) = 0.71069 ,μ = 0.735 mm-1,F(000) = 5368,Rint = 0.0699,R = 0.0505 and wR = 0.0707.Two independent Zn atoms are both coordinated by six N atoms from three phen ligands.π-π and C-H···π interactions among the L ligands and Zn(phen)3 cations,π-π and C-H···π interactions among the Zn(phen)3 cations and N-H···O hydrogen bonds among the L ligands and nitrate anions connect the whole structure into a 3-D supramolecular framework.     

Synthesis and Crystal Structure of a New Complex Zn(Ⅱ)L_2·2CH_3OH(H_2L = 4-Chloro-2-(2,3-dihydro-1H-benzoimidazol-2-yl)-phenol)

A new complex Zn(Ⅱ)L2·2CH3OH(H2L = 4-chloro-2-(2,3-dihydro-1H-ben-zoimi-dazol-2-yl)-phenol) has been prepared and characterized by single-crystal X-ray diffraction analysis and elemental analysis.The crystal is of triclinic system,space group P1 with a = 9.2905(10),b = 10.3555(13),c = 14.9590(14) ,α = 101.0340(10),β = 101.261(2),γ = 99.1660(10)o,V = 1356.1(3) 3,Z = 2,C28H24Cl2N4O4Zn,Mr = 616.78,Dc = 1.510 g/cm3,μ = 1.145 mm·1,F(000) = 632,the final R = 0.0379 and wR = 0.0830 for 3606 observed reflections with I 2σ(I).The Zn(Ⅱ) atom presents a distorted square pyramidal coordination involving two H2L ligands.The hydrogen bonds and π···π stacking interactions extend the complex into a two-dimensional framework.     

Isolation and Crystal Structure of Ent-kaurane Diterpenes from Rubus corchorifolius L. f.

In this study, ent-Kaurane-3β,16β,17-triol(1) and ent-kaurane-2α,16β,17-triol(2), were isolated from the leaves of Rubus corchorifolius L. f. Their structures were elucidated based on extensive spectroscopic analysis. NMR experiments identified the two compounds and X-ray crystallographic analysis confirmed their crystal structures. The crystal of 1 belongs to monoclinic with space group P21 and a = 10.7641(3), b = 7.2789(3), c = 11.7862(4) , β = 95.275(3)°, V = 919.55(6) 3, Z = 2, C20H34O4, Mr = 322.49 g/mol, Dc = 1.230 g/m3, F(000) = 376, λ = 1.54178 , μ = 0.661 mm-1, R = 0.0319, and wR = 0.0811 for 10889 observed reflections(Ⅰ 2σ(Ⅰ)). The crystal of 2 is classified as orthorhombic with space group P212121 and a = 10.7641(3), b = 12.72224(19), c = 21.3929(3) , V = 1748.94(4) 3, Z = 4, C20H34O4, Mr = 322.47, Dc = 1.225 Mg/m3 F(000) = 712, λ = 1.54184 , μ = 0.625 mm-1, R = 0.0303 and w R = 0.0759 for 10470 observed reflections(Ⅰ 2σ(Ⅰ)). Meanwhile, the compound revealed low inhibitory activities toward Hep G2, MCF-7, and SCG-7901 cells.     

Synthesis, Crystal Structure and Characterization of a New Mononuclear Zn（Ⅱ） Complex from Schiff-base Ligand

A new mononuclear [Zn（H-1L）2] （L = 1H-indole-3-ethylene-salicylaldimine） was synthesized through the reaction of Zn（Ac）2, salicylaldehyde and tryptamine in hot ethanol solution and characterized by X-ray crystal structure analysis. The crystal belongs to monoclinic, space group P21/n with a = 15.014（2）, b = 10.857（1）, c = 17.489（1）A,β = 95.49（1）°, V = 2837.8（5） A^3, Z = 4, Dc = 1.386 g/cm^3, μ = 0.904 mm-1, F（000） = 1232, the final R = 0.0463 and wR = 0.0890 for 4990 independent reflections. In the complex, the Zn2＋ ion presents a distorted N2O2 tetrahedral coordination involving two H-1L ligands.     

Synthesis, Crystal Structure and Fungicidal Activity of （Z）-3,3-Dimethyl-1-（1H-1,2,4-triazol-1-yl）butan-2-one O-2-Chlorobenzyl Oxime Nitrate

The title compound has been synthesized by the reaction of 3,3-dimethyl-1-(1H-1,2,4-triazol-1-yl)butan-2-one oxime with 2-chlorobenzyl chloride, and then treated with 65～68% HNO3. Its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 14.5481(8), b = 9.3351(5), c = 13.1911(7) , β = 98.9450(10)°, Z = 4, V = 1769.67(17) 3, Mr = 369.81, Dc = 1.388 g/cm3, S = 1.06, μ = 0.247 mm-1, F(000) = 776, the final R = 0.0352 and wR = 0.0960 for 3069 observed reflections (I > 2σ(I)). X-ray crystal structure presents the intramolecular N–H…O hydrogen bond. The packing is nearly parallel without π-π stacking interactions between two adjacent phenyl rings and stabilized by Van der Waals force. The preliminary bioassay shows that the title compound possesses fungicidal activity against Gibberella zeae at the dosage of 25 mg/L.     

Synthesis,Crystal Structure and Photoluminescence of a New Zn(Ⅱ) Dimer Constructed by 1,10-Phenanthroline Derivative and Flexible Dicarboxylate

A new compound,[Zn(L)(1,4-chdc)]2·2H2O(1,1,4-chdc = 1,4-cyclohexanedicarboxylate and L = 11-fluoro-dipyrido[3,2-a:2,3-c]phenazine),has been synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction.The crystal of 1 belongs to triclinic,space group P1 with a = 9.4679(19),b = 10.915(2),c = 12.577(3) ,α = 77.22(3),β = 74.73(3),γ = 65.47(3)°,C52H39F2N8O10Zn2,Mr = 1104.65,V = 1131.4(4) 3,Z = 1,Dc = 1.621 g/cm3,S = 1.091,μ(MoKα) = 1.143 mm–1,F(000) = 565,R = 0.0426 and wR = 0.1171.In 1,two 1,4-chdc anions bridge two Zn(Ⅱ) atoms to form a dimer.The neighboring dimers are further extended by π-π stacking interactions to form a 2D supramolecular layer.The luminescent property of the compound has also been investigated.     

Synthesis,Crystal Structure and Spectroscopic Properties of Zn(Ⅱ) with N-carbamylglutamate Ligand

Zn C6H8N2O5.H2O(NCGZn) has been synthesized, and its functional groups present in the title compound were confirmed by elemental analysis, TG and IR spectral studies. Meanwhile, the crystal of NCGZn was obtained by slow evaporation of a saturated aqueous solution at room temperature and confirmed by single-crystal X-ray diffraction analysis. It crystallizes in triclinic, space group P21 with a = 5.03220(1), b = 13.3747(4), c = 12.9944(4) , β = 92.987(2)o, V = 873.39(4) 3, Z = 2, C12H20N4O12Zn2, Mr = 543.10, Dc = 2.065 g/cm3, F(000) = 552, μ(Mo Ka) = 2.826 mm-1, R = 0.0422 and w R = 0.1142. In NCGZn, Zn(1) and the symmetry formed Zn(1) ions are connected by five atoms from four NCG-2H anions and a water molecule. A NCG ligand has two carboxylate groups, one connecting a Zn ion, and the other bridgiong two Zn ions. The NCG ligand bridges four Zn ions through the amino group and two carboxylate groups with a water molecule to yield a 3D coordination polymer structure with hydrogen bonds.     

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.     

Synthesis and Crystal Structure of 2-Methoxy-benzoic Acid 2-Oxo-3-（2,4,6-trimethyl-phenyl）-1-oxa-spiro[4.4]non-3-en-4-yl Ester

The new title compound 2-methoxy-benzoic acid 2-oxo-3-(2,4,6-trimethyl-phenyl)-1-oxa-spiro[4.4]non-3-en-4-yl ester(3,C25H26O5) has been synthesized by the condensation reaction of 4-hydroxy-3-(2,4,6-trimethyl-phenyl)-1-oxa-spiro[4.4]non-3-en-2-one(2) with 2-methoxylben-zoyl chloride,and characterized by 1H NMR and MS spectra.Its crystal structure was determined by single-crystal X-ray diffraction.The crystal is of monoclinic,space group P21/c with a = 10.6945(7),b = 12.8176(7),c = 16.4223(10) ,β = 103.5665(17)o,V = 2188.3(2) 3,Z = 4,Dc = 1.234 g/cm3,F(000) = 864.000,μ = 0.085 mm-1,the final R = 0.0520 and wR = 0.1132 for 2732 observed reflections with I 2σ(I).In the crystal structure,the C(1)-C(2)(1.478 ) bond is significantly shorter than the normal single C-C bond(1.53 ),suggesting that the carbonyl group on C(1) has formed a conjugated system with a double bond on C(2) and C(12).     

Synthesis,Crystal Structure and Antitumor Activity of 2-(3-Methyl-5-(methylthio)-4H-1,2,4-triazol-4-yl)isoindoline-1,3-dione

The title compound 2-(3-methyl-5-(methylthio)-4H-1,2,4-triazol-4-yl)isoindoline-1,3-dione(C12H10N4O2S, Mr = 274.30) has been synthesized by a three-step procedure including the cyclization, hydrazinolysis and substitution reactions, and its crystal structure was determined by X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 12.264(3), b = 14.646(3), c = 14.349(4) , β = 91.69(3)°, μ = 0.255 mm-1, Mr = 274.30, V = 2576.2(10) 3, Z = 8, Dc = 1.414 g/cm3, F(000) = 1136, R = 0.0487 and w R = 0.1329 for 4048 observed reflections with Ⅰ 2σ(Ⅰ). In addition, the preliminary bioassay suggested that the title compound 6 exhibits relatively good antitumor activity against HT-29 and MCF-7.     

Crystal Structure of a Cadmium（II） Complex Containing an Amide Type Ligand

The compound [Cd(L)2(NO3)]NO3·0.5H2O (L = N-benzyl-2-(quinolin-8-yloxy)aceta- mide) 1 has been synthesized and structurally determined by single-crystal X-ray diffraction, elemental analysis, IR and UV spectroscopy. The crystal belongs to the triclinic system, space group P1 with a = 11.7175(13), b = 11.8873(13), c = 14.0958(16) , α = 74.889(2), β = 78.228(2), γ = 78.831(2)o, V = 1835.0(4) 3, Z = 1, Dc = 1.502 Mg/m3, Mr = 1660.17,μ = 0.662 mm-1, F(000) = 846, λ(MoKα) = 0.71073 , the final R = 0.0585 and wR = 0.0577 for all observed reflections. The results show that the Cd(Ⅱ) ion with a square antiprismatic geometry is coordinated by a N2O6 donor set, two NO2 sets from two ligands and two O atoms from a bidendate nitrate group. In the crystal, the O-H···O and N-H···O hydrogen bonds are helpful to consolidate the three- dimensional network.     

Synthesis and Crystal Structure of a Palladium(II) Coordination Polymer [Na_2Pd(2,6-pydc)_2(H_2O)_6]_n

A novel coordination polymer [Na2Pd(2,6-pydc)2(H2O)6]n (2,6-H2pydc = 2,6-pyri- dinedicarboxylic acid) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c, with a = 11.962(2), b = 6.5552(13), c = 12.673(3) , β = 91.72(3)°, V = 993.3(3) 3, Z = 2, Mr = 590.68, Dc = 1.975 g/cm3, μ = 1.059 mm-1, F(000) = 592, the final R = 0.0211 and wR = 0.0454. In the crystal the Pd(II) ion adopts a distorted four-coordinated square-planar geometry and bonds to two bidentate 2,6-pyridinedicarboxylate molecules through caronyl oxygen and pyridine nitrogen atoms. The title complex exhibits a novel three-dimensional network structure.     

Semi-synthesis and Crystal Structure of Sophoridine N-oxide

Sophoridine N-oxide was synthesized and characterized by 1H-NMR,EI-MS,IR and elemental analysis,together with X-ray single-crystal diffraction analysis,and its crystal structure was reported for the first time.The crystal belongs to the orthorhombic system,space group P212121 with a = 8.321(2),b = 15.650(3),c = 24.352(5) ,V = 3171.1(11) 3,Z = 8,Dc = 1.258 g/cm3,λ(CuKα) = 1.54178,F(000) = 1440,the final R = 0.0351 and wR = 0.0970.The crystal structure shows Sophoridine N-oxide crystallizes with two host molecules of similar conformation and four water solvent molecules in the asymmetric unit.In the crystal structure,intermolecular O-H…O hydrogen bonds link the constituent molecules into a 2D layer structure,which further extends to a 3D supramolecular architecture via Van der Waals interactions and intermolecular O-H…O hydrogen bonds.     

The structure and dielectric properties of ionic compounds with flexible ammonium moiety

The 3-morpholin-4-yl-propyl-ammine tetrafluoroborate(MPA+)(BF4)(1) and the 3-morpholin-4-ylpropyl-ammine perchlorate(MPA+)(Cl O4)(2) were synthesized and separated as colorless block crystal.The(MPA+)(BF4) undergoes a reversible phase transition at ca.347.3 K with a hysteresis of16.1 K.Dielectric measurement also can confirm the transition.The crystal structure determined at300 K(monoclinic,P21/c,a = 9.978(2) ,b = 7.5206(15) ′,c = 15.058(3) ,b = 96.99(3)8,v = 1121.6(4)  3,z = 4) and 373 K(triclinic,P-1,a = 10.021(7) ,b = 7.662(3) ,c = 7.920(4) ,a = 95.012(14)8,b = 101.67(4)8,g = 91.48(3)8,v = 592.7(6) 3,z = 2) reveal that this compound has two phase.The most distinct is the BF4 anion is disorder at 373 K,which is probably the driving force of the phase transition.DSC measurement,dielectric measurement and the crystal structure of the compound 2 did not change at 300 K and 100 K.     

Synthesis and Crystal Structure of 3,3＇-Bis（2-benzimidazolyl）-2,2＇-dipyridine with Hydrated Zinc（Ⅱ） Perchlorate

The reaction of Zn(ClO4)2·6H2O with 3,3'-bis(2-benzimidazolyl)-2,2'-dipyridine (L) gave a mononuclear zinc(II) complex: [ZnL2](ClO4)2·2DMF·4H2O, which was structurally characterized by EA, IR, UV, 1H NMR, fluorescence spectrum and single-crystal X-ray diffraction. The crystal (C54H54Cl2N14O14Zn, Mr = 1259.38) belongs to the monoclinic system, space group C2/c with a = 20.874(2), b = 14.9953(16), c = 20.462(3) , β = 101.553(2)°, V = 6274.8(13) 3, Z = 4, Dc = 1.333 g/cm3, F (000) = 2608, μ(MoKα) = 0.548 mm–1, R = 0.0682 and wR = 0.1931 for 4984 observed reflections with I > 2σ(I). The Zn(II) is four-coordinated in a slightly distorted tetrahedral geometry through four N atoms from four benzimidazole units of two ligands. In the crystal lattice, the [ZnL2]2+ cations are linked to each other by extensive intermolecular hydrogen bonds between nitrogen atoms of benzimidazole rings, water and DMF molecules.     

Structure Analysis of Beta-alumina Synthesized by Solid State Reaction

The crystal structure of a solid electrolyte, beta-Al2O3, was investigated by XRD analysis and demonstrated by Diamond software. Its chemical formula was verified by the Ag ion molten salt exchange method and X-ray fluorescence analysis(XRF). The chemical formula of β-Al2O3 is Na2O·8.52Al2O3, and its crystal is of hexagonal, space group P63/mmc, with a = 5.5941  and c = 22.5300 . The chemical formula of β'-Al2 O is Na2O·6.03Al2O3, and its crystal is of trigonal, space group R 3 m, with a = 5.6017 and c = 33.6219 . The maximum span in the sodion migration of β'-phase(2.4283 ) is only about a third of that for the β'-phase(6.9037 ), so the β'-phase has higher ionic conductivity than the β-phase.     

Synthesis,Crystal Structure and Photoluminescence of a Three-dimensional Zinc(Ⅱ) Coordination Polymer with(20~3)_2(20)_3 Topology

The title compound,[Zn2(H2C4BIm)(ox)2]·2H2O(1,H2C4BIm = 2,2'-(1,4-bu-tanediyl)bis(1H-benzimidazole),has been synthesized by the hydrothermal reaction of Zn(NO3)2·6H2O with H2C4BIm and Na2C2O4 in water solution.It crystallizes in the triclinic system,space group P1 with a = 9.445(9),b = 9.598(9),c = 14.962(14) ,α = 72.160(10),β = 79.905(12),γ = 83.680(11)°,Mr = 633.18,V = 1269(2) 3,Z = 2,Dc = 1.657 g/cm3,F(000) = 644,μ = 1.953 mm-1,the final R = 0.0671 and wR = 0.1689.X-ray crystal structure analysis revealed that 1 is a 3D network with(203)2(20)3 topology in which the ZnII atom can be considered as a 3-connected node and both ox2-and H2C4BIm serve as the linear linkers.     

Synthesis and Crystal Structure of a Cu(Ⅱ) Coordination Polymer: [Cu(L)(1,10-phen)]_n

A new complex [Cu(L)(1,10-phen)]n(1, L = N-3-pyridine sulfonyl amino acid) has been synthesized and characterized by IR, elemental analysis and X-ray diffraction analysis, and its crystal belongs to monoclinic, space group P21/c with a = 11.481(2), b = 18.094(4), c = 8.5198(17) , β = 102.26(3)°,V = 1729.5(6) 3, Z = 4, Dc = 1.759 g/cm3, F(000) = 932, μ = 1.422 mm-1, R = 0.0368 and wR = 0.0893. In 1, the Cu(Ⅱ) ion adopts a slightly distorted five-coordinated square pyramidal geometry. The L2- ligand adopts O of the carboxyl bridging adjacent Cu(Ⅱ) units to form an infinite chain structure along the c axis. Also, π-π stacking interactions between the adjacent chains expanded the 1-D structures into a 3-D supramolecular structure.     

Synthesis and Crystal Structure of 7-Acetamido-5-chloro-8-（p-methyl- oxybenzenesulfonyloxy）-2-styrylquinoline

The title compound 7-acetamido-5-chloro-8-(p-methyloxybenzenesulfonyloxy)-2- styrylquinoline 4 (C26H21ClN2O5S, Mr = 508.96) has been synthesized and characterized by 1H- NMR, IR, ESI-MS and single-crystal X-ray diffraction techniques. The crystal belongs to orthorhombic, space group Pca21, with a = 7.920(3), b = 10.672(5), c = 28.008(12) , V = 2367.3(17) 3, Z = 4, Dc = 1.425 g/cm3, μ = 0.290 mm-1, F(000) = 1056, R = 0.0323 and wR = 0.0692 for 3895 unique reflections with 3127 observed ones (I > 2σ(I)). X-ray analysis reveals that the styrylquinoline subunit adopts a coplanar conformation, where the benzene ring and quinoline are in trans configuration.