Crystal Structure of 2-（2-Carboxy-4-hydroxy-6- methoxyphenoxy）-3,5-dichloro-6-hydroxy- 4-methylbenzoic Acid 1-Methyl Ester

The title compound, neogeodin hydrate （C17H14C1208, CAS： 94540-50-8）, was derived from marine fungus Aspergilhts terreus CRIM301. It was unequivocally characterized by IR, NMR spectroscopies, and single-crystal X-ray crystallography and tested for various biological activities. Neogeodin hydrate crystallizes in the triclinic space group P1 with a = 8.1159（5） A, b = 8.2472（4） A, c= 14.1278（7） A, a = 81.448（2）°, β = 84.860（2）°, γ= 70.400（2）°, V = 880.13（8） A3; Z = 2. It comprises a diphenyl ether, asterric acid skeleton and dichloro substituents. The methoxyphenoxy rings of the inversely related molecules form a ribbon-like structure that is stabilized by O-H...O hydrogen bonds through the doubly disordered carboxyl groups and by C-H...O interactions, generating the same R22（8） ring motif. The chlorinated methylbenzoate rings, making mostly a right angle, link the parallel upper and lower ribbons via bifurcated O-H...O and C-H...O hydrogen bonds, yielding endless channels. The channels formed are further sustained by C-H...O and π...π interactions Neogeodin hydrate exhibits inhibition against superoxide anion radical formation in the xanthine/xanthine oxidase （XXO） assay, but has no aromatase inhibitory activity.     

Synthesis and Crystal Structure of 1,4,7,10-Tetrakis （2-（（4-hydroxy）phenoxy）ethyl）-1,4,7,10- tetraazacyclododecane

A novel molecule tetra-N-alkylation of cyclen （1,4,7,10-tetraazacyclododecane）, 1,4,7,10-tetrakis（2-（（4-hydroxy）phenoxy）ethyl）-1,4,7,10-tetraazacyclododecane 2, was synthesized and structurally characterized by single-crystal X-ray diffraction. The molecule turned into chiral helical compound crystals grown from EtOH by slow diffusion at room temperature and three of the four hydroquinone groups of the benzene ring formed a g-electron-rich cavity by C-H…π stacking interaction. The crystal belongs to the monoclinic system, space group P21/C with a = 13.9192（9）, b = 13.2871（6）, c = 22.1894（15）A^°, β = 91.4600（10）°, V = 4102.5（4）A^°3, Z = 4, Dc = 1.219 g/cm^3, C40H52N4O8, Mr = 752.89, F（000） = 1616,μ = 0.088 mm^-1, MoKa radiation （λ = 0.71073）, R = 0.0578 and wR = 0.1389 for 5588 observed reflections with I 〉 2σ（I）. Moreover, compound 2 was characterized with ^1H NMR, ^13C NMR, IR spectra and MS.     

A Potassium Organic-inorganic Hybrid Complex with Channels Hosting Decorated Poly-anion Chains

A potassium organic-inorganic hybrid complex {H2[K（PMo12O40）（CH3CN）3]- （dpdo）2（H2O）}n 1 （dpdo = 4,4＇-bipyridine-N,N＇-dioxide） with special channels for the chain-like assembly of decorated Keggin-type anions was synthesized and structurally characterized. The crystal structure was determined by single-crystal X-ray diffraction. The crystal is of orthorhombic, space group Cmcm with a = 20.5328（17）, b = 16.8877（14）, c = 16,1454（14） A, V = 5598.4（8） A^3, Z = 4, C26H29N7O45KMo12P, Mr= 2380.91, Dc = 2.825 g/cm^3,μ = 2.813 mm^-1, F（000） = 4528, the final R = 0.0324 and wR = 0.0880 for 2577 observed reflections with I 〉 2σ（I）. Compound 1 exhibits a 3D network structure with large channels hosting decorated poly-anion chains as guests.     

Synthesis and Structure of a La（Ⅲ） Complex of 1,10-Phenanthroline-2,9-dicarboxylate： a Three-dimensional Network via Hydrogen Bonding Interactions

A new La（Ⅲ） complex, {[La（L）（NO3）（H2O）3]·H2O}n （L = 1,10-phenanthroline- 2,9-dicarboxylate）, has been synthesized and structurally determined by X-ray diffraction analysis. The complex crystallizes in the monoclinic system, space group P21/c with a = 7.7358（17）, b = 8.1664（18）, c = 28.271（6） A, β= 95.184（4）°, V= 1778.6（7） A3, Z = 4, C14H14LaN3O11, Mr = 539.19, Dc = 2.014 g/cm^3, μ= 2.471 mm^-1, F（000） = 1056, the final R = 0.0350 and wR = 0.0659. In this complex, each metal center adopts a ten-coordination geometry formed by two N atoms from a ligand L and eight O atoms from three H2O molecules, a nitrate ion and carboxylates of two ligands. Each ligand adopts a N2,O3-pentdentate coordination mode using two N and two O atoms chelating a La（Ⅲ）, and using another O atom of carboxylate to bridge another La（Ⅲ） center resulting in a 1D helical chain molecule. Intermolecular strong O-H…O and weak C-H…O hydrogen bonds extend the 1D chain structure into a 3D supramolecular architecture.     

Synthesis,Crystal Structure and Antibacterial Activity of （E）-N1,N4-Bis（2,3,4-trimethoxy-6- methylbenzylidene）butane- 1,4-diamine

The title compound （E）-N1,N4-bis（2,3,4-trimethoxy-6-methylbenzylidene） butane- 1,4- diamine （C26H36N2O6, Mr = 472.57） was synthesized and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. The crystal belongs to triclinic, space group C2/c with a = 36.102（4）, b = 5.6620（11）, c = 13.015（2）A,β = 105.491 （2）°, V = 2563.7（7）A3, Z = 4, Dc = 1.224 g/cm3, 2 = 0.71073 A,μ（MoKα） = 0.087 mm^-1, F（000） = 1016, the final R = 0.0456 and wR = 0.1257 for 2255 observed reflections with I 〉 2σ（I）. X-ray diffraction analysis reveals that the molecule adopts an E configuration about the central C=N functional bond. The phenyl rings of two 2,3,4-trimethoxy-6-methylbenzaldehyde groups are parallel by symmetry. The molecules are linked through π-π and C-H…π stacking interactions and C-H…O hydrogen bonding interactions. The title compound possesses moderate antibacterial activity.     

Synthesis and Crystal Structure of a 1D Coordination Polymer： {[Cu（HSSA）（py）3]·H2O}n （H3SSA = 5-Sulfosalicylic Acid,py = Pyridine）

The title compound [Cu（HSSA）（py）3H2O]n （H3SSA = 5-sulfosalicylic acid, py = pyridine） I has been synthesized and structurally determined by single-crystal X-ray diffraction. I was further characterized by elemental analyses, thermogravimetric analyses, IR and UV-visible spectroscopy. The crystal belongs to the monoclinic system, space group P21/c with a = 9.4564（10）, b = 18.2679（19）, c = 15.7284（12） A,β= 126.045（4）°, V= 2196.9（4）A^3, Z= 4, Dc = 1.618 g/cm^3, Mr = 535.02,μ = 1.141 mm^-1, F（000） = 1100, 2（MoKα） = 0.71073 A, the final R = 0.0429 and wR = 0.1044 for all observed reflections. In the structure, every two Cu（II） atoms are bridged by a bivalent 5-sulfosalicylic anion to form a 1D chain-like coordination polymer. Lattice waters between chains link them to form 2D layers which are further linked by C-H…O hydrogen bonds to form a three-dimensional supramolecular network.     

Synthesis, Crystal Structure and Binding Properties of 6H,7H,13H,14H-5a,6a,7a,12a,13a,14a- Hxaazbenz[f]indeno[2,1,8-ija]naphth[2,3- f]azulene-14b,14c-dicarboxylic-5,8,12,15- tetrahydro-6,8,14-trioxo-diethyl Ester

The title compound 6H,7H,13H,14H-5a,6a,7a,12a,13a,14a-hxaazbenz[f]indeno[2,1,8- ija]naphth[2,3-f]azulene- 14b, 14c-dicarboxylic-5,8,12,15-tetrahydro-6,8,14-trioxo-diethyl ester （C27H26N6OT, Mr = 546.54） has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P211c with a = 8.8129（6）, b = 17.9883（13）, c = 16.2623（11）A, β = 98.770（2）°, V = 2547.9（3）A3, Z = 4, De= 1.425 g/cm3, p（MoKa） = 0.105 mm-1, F（000） = 1144, the final R = 0.0672 and wR = 0.1162 for 2275 observed reflections with I 〉 2σ（I）. The crystal structural analysis shows that intermolecular C-H...O hydrogen bonds and π-π stacking interactions result in a three-dimensional framework. The binding study by fluorescence spectroscopy titration showed that he title compound can selectively recognize Fe3＋ with fluorescence quenching.     

Synthesis and Crystal Structure of 4-（2-Bromophenyl）-3,4,7,8-tetrahydro- 7,7-dimethyl-1-p-tolylquinoline-2,5（1H,6H）-dione

The title compound 4-（2-bromophenyl）-3,4,7,8-tetrahydro-7,7-dimethyl-1-p-tolylquinoline-2,5（1H,6H）-dione 1 （C24H24BrNO2, Mr = 438.35） was synthesized and characterized by IR, 1H NMR and elemental analysis. The crystal belongs to monoclinic, space group C2/c with a = 27.565（14）, b = 10.079（5）, c = 15.917（8） A,β = 111.059（9）°, Z = 8, V = 4127（4）A3, Dc = 1.411 g·cm^-3,μ（MoKa） = 2.011 mm^-1, F（000） = 1808, the final R = 0.0417 and wR = 0.1032 for 2393 observed reflections （I 〉 2σ（I））. X-ray analysis reveals that the pyridine ring adopts a distorted boat conformation, while another six-membered ring takes a half-chair conformation. In addition, there are non-classical hydrogen bonds of C-H…O and C-H…Br in the structure. The short distance （3.481A） between the adjacent 2-bromophenyl rings indicates the existence of π-π interaction.     

A Novel Palladium（II） Complex Self-assembled from Anthracene-9-carboxylic Acid： Synthesis, Crystal Structure and Spectroscopic Properties

A novel palladium（II） complex [（TMEDA）Pd（anca）2].2DMSO （1, TMEDA = N,N,N＇,N＇-tetramethylethylethylenediamine, anca = anthracene-9-carboxylic acid） was synthesized and characterized by single-crystal X-ray diffraction, 1H NMR, UV-Vis and fluorescence spectroscopy. The cell belongs to orthorhombic Aba2 space group with a = 19.698（7）, b = 21.045（7） c = 9.062（3） A, Z = 4, V= 3757（2） A3, C40H46N206PdS2, Mr = 821.31, D, = 1.452 g/cm3, F（000） = 1704, the final R = 0.0272, wR = 0.0667 and GOOF = 0.999. Complex 1 exhibits an interesting distorted clip-shaped molecular configuration which is stabilized by intramolecular C-H...O hydrogen bonds. The cells are packed into a 3D supramolecular structure based on the intermolecular C-H...zr interactions which further construct the tubular channels serving as guest molecular channels to include the DMSO solvent molecules inside. Furthermore, the spectroscopic properties of 1 were also investigated.     

Synthesis,Crystal Structure and Luminescent Property of [Zn（C12H9O3）2（C10H8N2）]n·nH2O

Under hydrothermal condition, the reaction of 2-naphthoxyacetic acid with ZnCl2 and 4,4′-bipyridine （4,4′-bipy） has afforded a new Zn（Ⅱ） compound, [Zn（C12H9O3）2（C10H8N2）]n·nH2O1, which was structurally characterized by single-crystal X-ray diffraction analysis. The crystal is of monoclinic, space group P21/c with a = 7.7335（2）, b = 19.3834（4）, c = 20.1707（4） A, β = 104.9830（10）°, V = 2920.82（11） A^3, C34H28ZnN2O7, Mr = 641.95, Z = 4, Dc = 1.460 g/cm^3,μ = 0.895 mm^-1, F（000） = 1328, R = 0.0406 and wR = 0.0876 for 4417 observed reflections （I〉 2σ（I）） Complex 1 consists of one-dimensional zigzag chains deriving from Zn（C12H9O3）2 units linked by 4,4′-bipy ligands, and lattice water molecules decorate between the chains. Non-covalent interactions, such as hydrogen-bonding and aromatic π-π interactions, lead to the formation of a 3D network structure. The thermogravimetric analysis （TGA） and luminescent property for 1 have also been studied in this paper.     

Synthesis and Crystal Structure of a Novel Three-dimensional Supramolecular Compound [（AgI3）（4-HBPFA）2（H2O）]

1 INTRODUCTION In recent years, the rational design and synthesisof metal-directed supramolecular frameworks throughintermolecular hydrogen bonds, π-π stacking interac-tion or other weak interactions have received muchattention because of their interesting molecular topo-logies and various potential applications in catalysis,superconductor, magnetism, nonlinear optics, sen-sors and molecular recognition[1～4]. On the otherhand, the attachment of mono- or polypyridyl frag-ments to a ferr…     

Synthesis and Crystal Structure of the Optical Activity of （Z）-Nitromethylene Neonicotinoid Analogue

A novel (Z)-nitromethylene neonicotinoid analogue (C23H27Cl2N5O4·2H2O) (II) with optical activity has been synthesized, the structure was characterized by elemental analysis, IR and 1H NMR spectra, and the (Z)-configuration was confirmed by single-crystal X-ray diffraction. The crystal belongs to triclinic, space group P1 with a = 7.4638(3), b = 12.6232(5), c = 15.2990(6), α = 71.907(1), β = 89.397(2), γ = 80.314(1)°, V = 1349.28(9)3, Z = 2, Dc = 1.340 g/cm3, μ = 0.286 mm-1, Mr = 544.43, F(000) = 572, S = 1.056, R = 0.0801 and wR = 0.2366 for 4998 unique reflections with 3012 observed ones (I > 2σ(I)). In the crystal, the dihedral angle between the pyridine and 4-Cl-phenyl rings is 58.13°. Intermolecular O–H···O, C–H···O and C–H···Cl hydrogen bonds involving water molecules stabilize the crystal structure.     

Structures of 1-（3,4-Dihydroxyphenyl）-2-（3,4-dimethoxyphenyl） ethanone and Its Hydrate Complex

The title compounds, C16H16O5 (I) and C16H16O5·H2O (II), were structurally characterized by single-crystal X-ray diffraction. Compound I crystallizes in monoclinic space group P21/c with a = 10.5574(10), b = 8.3576(9), c = 16.5528(16) , β = 91.762(3)°, Z = 4, R = 0.0524 and wR = 0.1084. The molecules are jointed into a chain by intermolecular O-H···O and C-H···O hydrogen bonds, which form layers parallel to (001). The chains run along the [110] and [110] directions alternatively layer by layer, and are assembled into a network by intermolecular O-H···O (carboxyl) hydrogen bonds. On the other hand, the hydrate complex (II) crystallizes in the triclinic space group P1 with a = 5.1451(2), b = 10.4583(4), c = 14.8267(5) , α = 70.900(2), β = 82.478(2), γ = 81.359(2)°, Z = 2, R = 0.0393 and wR = 0.0983. The molecules are linked into infinite two-dimensional ribbons by O-H···O (carbonyl) and solvent-bridged O-H···O hydrogen bonds.     

Synthesis and Structure of a La(Ⅲ) Complex of 1,10-Phenanthroline-2,9-dicarboxylate:a Three-dimensional Network via Hydrogen Bonding Interactions

A new La(Ⅲ) complex, {[La(L)(NO3)(H2O)3]·H2O}n (L = 1,10-phenanthroline- 2,9-dicarboxylate), has been synthesized and structurally determined by X-ray diffraction analysis. The complex crystallizes in the monoclinic system, space group P21/c with a = 7.7358(17), b = 8.1664(18), c = 28.271(6) , β = 95.184(4)°, V = 1778.6(7)3, Z = 4, C14H14LaN3O11, Mr = 539.19, Dc = 2.014 g/cm3, μ = 2.471 mm–1, F(000) = 1056, the final R = 0.0350 and wR = 0.0659. In this complex, each metal center adopts a ten-coordination geometry formed by two N atoms from a ligand L and eight O atoms from three H2O molecules, a nitrate ion and carboxylates of two ligands. Each ligand adopts a N2,O3-pentdentate coordination mode using two N and two O atoms chelating a La(III), and using another O atom of carboxylate to bridge another La(III) center resulting in a 1D helical chain molecule. Intermolecular strong O–H···O and weak C–H···O hydrogen bonds extend the 1D chain structure into a 3D supramolecular architecture.     

Synthesis and Crystal Structure of 4-Oxo-1,2,4-triazino[4,5-a]benzimidazole

The title compound 4-oxo-1,2,4-triazino[4,5-a]benzimidazole(C9H6N4O,Mr = 186.18) has been synthesized and structurally characterized by IR,NMR and single-crystal X-ray diffraction. The crystal belongs to monoclinic,space group P21/c,with a = 9.1530(18) ,b = 7.2260(14),c = 12.604(3) ,β = 106.92(3) ,V = 797.5(3) 3,Z = 4,Dc = 1.551 g/cm3,λ(MoKa) = 0.71073,F(000) = 384,μ(MoKa) = 0.109 mm-1,the final R = 0.0632 and wR = 0.1095. A total of 1444 unique reflections were collected,of which 767 with I > 2σ(I) were observed. The structure of the title compound is planar. In packing,the molecules are intersected to each other to form chains along three dimensions,together by intermolecular N-H…O and C-H…N hydrogen bonds. The whole structure is further stabilized by π…π interaction between two adjacent tricyclic ring systems,with the centroid-to-centroid distance of 3.369(4) .     

C-H…O Hydrogen Bonds and π…π Interaction and the Crystal and Molecular Structures of 3-Nitro-benzylideneaniline-methyl-2’

The title compound (C14H12N2O2,Mr=240.26) crystallizes in the monoclinic system,space group P21/a with a=7.394(1),b=21.334(3),c=7.423(1)A,β=89.82(1)A°,V=1170.8(3)A3,Z=4,Dc=1.363 g/cm3,μ(MoKα)=0.93 cm-1 and F(000)=504.00.The final R and wR are 0.0440 and 0.1370 for 2153 observed reflections (I>2σ(I)),respectively.The dihedral angle between the two phenyl rings is 52.9°and that between the NO2 group and its attached ring is 3.0°.In the crystal,molecules are stacked along [100] throughπ…πinteractions.The C-H…O hydrogen bond (3.403 A,120.4°) laterally connects the stacks along [010] to form networks (001) which are further anti-parallelly connected by C-H…O(3.382 A,142.9°) andπ…πinteractions extending along [001].Also presented here is a brief study on the C-H…O hydrogen bonds in nitro-substituted benzyl-ideneanilines which can be classified into five types,namely,R12(5)R21(4),R22(8),R12(6),andR22(7),with the first three occurring more often.     

Hydrothermal Synthesis and Crystal Structure of a New Polyoxovanadate: [Mn(en)3]2en0.5[HV8VV8IVO38(Cl)]·4.5H2O (en = Ethylenediamine)

A new compound has been synthesized under hydrothermal conditions and characterized by IR, elemental analysis, XPS and single-crystal X-ray diffraction analysis. The title compound [Mn(en)3]2en0.5[HV16O38(Cl)]·4.5H2O crystallizes in monoclinic, space group C2/c, with a = 17.016(4), b = 18.858(4), c = 18.872(4) (A), β = 93.667(4)°, V = 6043(2) (A)3, Z = 4, Dc = 2.242 g/cm3, Mr = 2040.12, F(000) = 4020, μ = 2.895 mm-1, Rint = 0.0921, R = 0.0649 and wR = 0.1325. Single-crystal X-ray structure analysis indicates that the title compound consists of a polyanion [HV8VV8IVO38(Cl)]4( cage, two [Mn(en)3]22 cations, four and a half lattice waters and a half ethylenediamine. In addition, intermolecular O-H…N,O-H…O and C-H…O and C-H…O hydrogen bonds link the molecules together to form a three-dimensional structure.     

Synthesis and Crystal Structure of a Novel Binuclear Cu(Ⅱ) Complex with Tetradentate Schiff-base Ligand

A novel binuclear complex ([Cu2(μ2-shed)(hshed)]·(ClO4)·H2O, h2shed = N-salicylidene-N′-(2-hydroxyethyl)ethylenediamine) has been synthesized and structurally characterized by X-ray diffraction analysis. It crystallizes in monoclinic, space group P21/c with a = 12.511(10), b =15.750(12), c = 14.281(12) (A), β = 100.564(14)°, C22H31ClN4O9Cu2, Mr = 658.04, V= 2766(4) (A)3, Z =4, Dc = 1.580 g/cm3, μ(MoKα) = 1.689 mm-1, F(000) = 1352, the final R = 0.0528 and wR = 0.1433 for 4880 independent reflections with Rint = 0.0577. The complex is a binuclear copper compound,and two Cu(Ⅱ ) ions in the binuclear cation are in different coordination environments. The Cu(1) ion adopts a distorted square pyramidal geometry (τ = 0.22) with four donor atoms (N2O2) of the ligand in the basal plane, and one hydroxyl oxygen atom with protonated form occupying the apical position.The Cu(2) ion assumes the geometry of a distorted square plane with four donor atoms (N2O2) of the ligand. The Cu…Cu separation is 3.103 (A). In addition, N-H…O and C-H…O intermolecular hydrogen bonding interactions link these binuclear cations into a quasi one-dimensional chain along the a axis.     

Synthesis and Crystal Structure of a 1D Coordination Polymer: {[Cu(HSSA)(py) 3]·H2O}n (H3SSA=5-Sulfosalicylic Acid, py=Pyridine)

The title compound [Cu(HSSA)(py)3H2O]n (H3SSA = 5-sulfosalicylic acid,py = pyridine) Ⅰ has been synthesized and structurally determined by single-crystal X-ray diffraction. Ⅰ was further characterized by elemental analyses,thermogravimetric analyses,IR and UV-visible spectroscopy. The crystal belongs to the monoclinic system,space group P21/c with a = 9.4564(10),b = 18.2679(19),c = 15.7284(12) ,β = 126.045(4)o,V = 2196.9(4) 3,Z = 4,Dc = 1.618 g/cm3,Mr = 535.02,μ = 1.141 mm-1,F(000) = 1100,λ(MoKα) = 0.71073 ,the final R = 0.0429 and wR = 0.1044 for all observed reflections. In the structure,every two Cu(Ⅱ) atoms are bridged by a bivalent 5-sulfosalicylic anion to form a 1D chain-like coordination polymer. Lattice waters between chains link them to form 2D layers which are further linked by C-H···O hydrogen bonds to form a three-dimensional supramolecular network.     

Synthesis and Crystal Structure of Bis{2-bromo- 4-chloro-6-[(2-isopropylammonioethylimino)-methyl]phenolato}bisthiocyanatozinc(Ⅱ)

A Schiff base zinc(Ⅱ) complex [Zn(C12H16BrClN2O)2(NCS)2] was prepared and characterized by elemental analysis, IR and single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P with a = 8.414(1), b = 9.124(1), c = 22.212(3) (A), α = 79.177(2), β = 86.296(2), γ = 89.899(2)o, V = 1671.3(4) (A)3, Z = 2, Dc = 1.631 g/cm3, Mr = 820.79, λ(MoKα) = 0.71073 (A), μ = 3.444 mm-1, F(000) = 824, R = 0.0646 and wR = 0.1179. A total of 7371 unique reflections were collected, of which 3904 with I＞2σ(I) were observed. The complex crystallizes with two half-molecules per asymmetric unit and each mononuclear molecule is centrosymmetric. The Zn atom lying at the inversion centre is six-coordinated in a slightly distorted octahedral geometry by two phenolate O atoms and two imine N atoms from two Schiff base ligands, as well as two N atoms from two thiocyanate anions. In the crystal structure, the combination of π-π stacking interactions and intermolecular hydrogen bonds (N-H…Br, N-H…O, N-H…N, C-H…O, C-H…S and C-H…Cl) leads to a three-dimensional network.