Syntheses, Structures and Luminescent Properties of Two Zinc Complexes Containing N-P-Acetamidobenzenesulfonyl-glycine Acid Ligand

Using N-P-acetamidobenzenesulfonyl-glycine acid （abbreviated as abglyH2） as a ligand, two zinc（II） complexes [Zn（abglyH）2（bipy）2（H2O）2], （1） and {[Znz（abgly）2（bipy）2（H2O）2]. 2（H2O）}n （2） （bipy = 4,4＇-bipyridine） have been synthesized under mild conditions and characterized by IR, elemental analysis and X-ray diffraction analysis. Complex 1 is a monomeric compound, which is further assembled by intermolecular hydrogen bonds and π-π interactions into a 3-D supramolecular network. Complex 2 adopts a one-dimensional double chain structure and is further linked by hydrogen bonds to form a 2-D structure. Fluorescent analysis shows that complex 1 has an emissive maximum at 337 nm and complex 2 exhibits an emissive maximum at 339 nm in the solution state at room temperature.     

Syntheses, Structures and Luminescent Property of Two Supramolecular Complexes Containing N-P-Acetamidobenzenesulfonyl-glycine Acid Ligand

Making use of N-P-acetamidobenzenesulfonyl-glycine acid （abbreviated as abglyH2）,two transitional metal complexes [Zn（abglyH）（phen）2]ClO4·H2O （1） and Co（abglyH）2（bipy）2（H2O）2 （2） （phen = 1,10-phenanthroline,bipy = 4,4＇-bipyridine） have been synthesized under mild conditions and characterized by IR,elemental analysis and X-ray diffraction analysis. Complex 1 is a monomeric compound which is further assembled by intermolecular hydrogen bonds and π-π interaction into a 2-D supramolecular network. Complex 2 is also a monomeric compound and further connected by intermolecular hydrogen bonds to form a 2-D supramolecular network. Fluorescent analysis shows that complex 1 has an emissive maximum at 364 nm in the solution state at room temperature.     

Synthesis and Crystal Structure of Sodium Monosulfuron （N-（4-Methylpyrimidin-2-yl）-N＇-2-（nitrophenylsulfonyl） Urea Sodium）

ABSTRACT Monosulfuron is a novel sulfonylurea herbicide with ultra-low dosage invented and patented by Nankai University. Herein its sodium salt was firstly synthesized and crystal structure was determined by X-ray diffraction method. The title compound belongs to the triclinic system, space group P1^- with a = 7.306（6）, b = 9.446（8）, c = 11.872（10）A, α = 76.578（14）, β = 78.049（13）, γ = 77.620（14）°, V = 767.7（11）A^3, Mr = 377.32, Z = 2, Dc = 1.632 g/cm^3,μ= 0.283 mm^-1, F（000） = 388, R = 0.0444 and wR = 0.1186. In the title compound, Na（1） coordinates with 0（4） and 0（5） from one monosulfuron molecule, N（4A） and O（5A） from the other monosulfuron molecule and the oxygen atom from H2O to give five coordination bonds. The title complex is further linked into a three-dimensional structure through π…π interactions and intermolecular hydrogen bonds between the oxygen and nitrogen atoms.     

Synthesis,Crystal Structure and Biological Activities of N-（4-Cyanopyrazole-3-yl）- α-（3,5-difluorophenyl）- O,O-diisopropyl- α-aminophosphonate

The title compound has been synthesized by the addition reaction of N-（4-cyanopyrazole-3-yl）-3,5-difluorophenyl-imine and diisopropyl phosphate. Its structure was confirmed by means of IR, ^1H NMR and elemental analysis. The single-crystal structure of the title compound was determined by X-ray crystallography. The compound crystallizes in monoclinic, space group C2/c with a = 18.9959（14）, b = 9.2212（7）, c = 22.1108（16）A^°, β= 90.1540（10）°, V = 3873.0（5） A^°^3, Dc = 1.366 g/cm^3, Z = 8, μ = 0.185, F（000） = 1664, and the final R = 0.0503 and wR = 0.1539 for 2996 observed reflections （I 〉 2σ（I））. The results demonstrate that the dihedral angle between the pyrazole and benzene rings is 105.5°, and there is a full delocalized pyrazole system with sp^2 hydridization of N（3）. The crystal structure is stabilized by two intermolecular hydrogen bonds of N（1）-H（1）…O（3） and N（3）-H（3A）…N（4）. The preliminary biological test shows that the title compound has a moderate antifungal activity.     

Synthesis and Crystal Structure of 5,7-Dimethoxy-2-phenylquinolin-4-yl Phenyloxy （N-L-Alanine ethyl ester） Phosphoramidate

5,7-Dimethoxy-2-phenylquinolin-4-yl phenyloxy （N-L-alanine ethyl ester） phosphoramidate （C28H29N2O7P, Mr = 536.17） has been synthesized by a facial phosphorylated reaction, and its structure was determined by IR, NMR, HR MS and X-ray single-crystal diffraction. The crystal belongs to triclinic, space group P1^-, with a = 11.375（2）, b = 11.591（2）, c = 11.638（2） A^°, α= 109.46（3）, β= 104.58（3）, γ= 100.48（3）°, V = 1339.6（5）A^°^3, Z = 2, Dc = 1.330 g/cm^3,μ = 0.152 mm^-1, F（000） = 564, the final R = 0.0654 and wR = 0.1546. In the crystal structure, the title compound is constructed by a centrosymmetric dimmer unit composed of a pair of π-π stacking diastereoisomers. The compound has a noteworthy feature in the framework, and such units are linked by two equal intermolecular P=O…H-N hydrogen bonds.     

A Facile Synthesis and Crystal Structure of 1-Amino-3-（2′-methylphenyl）isoquinolin Hydrochloride

The title compound （C16H15ClN2） has been synthesized by a facile self-condensation of o-tolunitrile promoted by potassium tert-butanolate in DMPU, and its structure was characterized by ^1H NMR, ^13C NMR, IR, UV, HRMS and X-ray single-crystal diffraction. The crystal belongs to orthorhombic, space group Pna21 with a = 19.560（3）, b = 7.8500（14）, c = 18.428（3） A^°, Dc = 1.271 g/cm^3, Z= 8, 2 = 0.71073 A^°,μ（MoKa） = 0.257 mm^-1, Mr = 270.75, V= 2829.5（8） A^°^3, Flack parameter = 0.12（12）, F（000） = 1136, the final R = 0.0571 and wR = 0.1445 for 2701 observed reflections with I 〉 20（I）. The intermolecular N-H…Cl hydrogen bonds link the molecules into a one-dimensional chain running along axis a.     

Hydrothermal Synthesis and Crystal Structure of a Novel Polyoxometalate K（C4N2H12）4（C4N2H11）2- [Mo8^VMo4^（VI）CdP8O54（OH）8]F·6H2O

The title compound 1 has been synthesized by the reaction of H2MoO4,CdCl2,H3PO4,KF,piperazine hexahydrate and water in aqueous solution under mild hydrothermal conditions. Single-crystal X-ray analysis reveals that the title compound crystallizes in the triclinic system,space group P1 with a = 14.049（3）,b = 15.972（3）,c = 20.043（4） A,α = 85.82（3）,β = 81.28（3）,γ = 67.15（3）°,V = 4095.9（14） A^3,Mr = 3204.62,Z = 2,Dc = 2.598 g/c^m3,μ = 2.360 mm^-1,F（000） = 3124,the final R = 0.0314,wR = 0.0826 and S = 0.989 for 18592 observed reflections with I 〉 2σ（I）. The crystal packing is stabilized by N–H… and O–H… intraand intermolecular hydrogen bonds to form an infinite 3D network.     

Hydrothermal Synthesis and Crystal Structure of a New Polyoxovanadate： [Mn（en）3]2en0.5[HV8VV8IVO38（CI）]·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[HV8VV8IVO38（CI）]·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）A3, 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（CI）]4- cage, two [Mn（en）3]2^2＋ cations, four and a half lattice waters and a half ethylenediamine. In addition, intermolecular O-H...N, O-H...O, N-H...O and C-H...O hydrogen bonds link the molecules together to form a three-dimensional structure.     

Isolation, Crystal Structure and Inhibitory Activity against Magnaporthe Grisea of （2R,3R）-3,5,7-trihydroxyflavanone 3-Acetate from Myoporum Bontioides A. Gray

The title compound, (2R,3R)-3,5,7-trihydroxyflavanone 3-acetate, is a flavanonol derivative which was first isolated from Myoporum bontioides A. Gray and characterized by MS, NMR and CD spectra. In addition, the structure was determined by X-ray single-crystal diffraction analysis. It crystallizes in the triclinic lattice, space group P21 with a = 10.686(3), b = 6.862(2), c = 11.267(3) , β = 107.46(1), V = 788.3(4) 3, Z = 2, C17H16O7, Mr = 332.30, Dc = 1.400 g/cm3, μ(MoKα) = 0.110 mm-1, F(000) = 348, the final R = 0.0283 and wR = 0.0826 for 3428 independent reflections (Rint = 0.017) and 1500 observed ones (I > 2σ(I)). The structure consists of one flavone and one water molecule. The flavone molecules form a 1D column by the p…π stacking interactions and C–H…O hydrogen bonds. The weak intermolecular/intermolecular O–H…O hydrogen bonds observed in the crystal give further rise to a complicated network structure. Primary bioassay showed that the title compound has high inhibitory activity against Magnaporthe grisea with the EC50 values of 199.41 μg/mL.     

A Photoluminescent Bimetallic Zinc-pyridinedicarboxylate：Diverse Supramolecular Motifs from Distinct Hydrogen Bonds

A cyclic bimetallic metal-organic complex [Zn（C）（H-fmpdc）（H2O）]2·2H2O （fmpdc = 4-（furan-2-yl）-2,6-dimethylpyridine-3,5-dicarboxylate） was synthesized and characterized by single-crystal X-ray analysis. The compound crystallizes in orthorhombic, space group Pbca with a = 12.905（2）, b = 14.774（3）, c = 16.833（3）A, V= 3029.4（10）A^3 Z = 4, Dc = 1.644 g/cm^3, F（000） = 1616, R = 0.0347 and wR = 0.0956 （I 〉 2σ（I））. There exist diverse supramolecular motifs （1-D, 2-D and 3-D） from distinct hydrogen bonds in the crystal structure of the title compound. The furanyl group has obvious contribution to the red-shift in the photoluminescent spectrum of the H2fmpdc ligand. The title compound 1 shows strong photoluminescence with emission maximum at 2 = 402 nm （λex.max = 367 nm）.     

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 and Crystal Structure of 1-[（1＇-Phenyl-5＇-methyl-4＇-pyrazolcarbonyl）-3-methylthio-5-amino-1Hy l-1,2,4-triazole

The title compound (C14H14N6OS, Mr=314.37) has been synthesized and characterized by IR, ^1H NMR and X-ray single-crystal diffraction techniques.The crystal structure shows the presence of a dimmer with intermolecular N(4)H(4)…N(3) hydrogen bonds.     

Synthesis and Crystal Structure of N-（1′-H-Pyrrol- 2′-ylcarbonyl）-5-amino- 1,10-phenanthroline

The title compound, N-（1′-H-pyrrol-2′-ylcarbonyl）-5-amino-1,10-phenanthroline, was synthesized by the reaction of a-pyrrolyl carbonyl chloride and 5-amino-1,10-phenanthroline in pyridine. Determined by X-ray structure analysis, it crystallizes in triclinic system, space group P1 with the following crystallographic data： C20H21N5O3, Mr = 379.42, a = 7.8559（4）, b = 9.1681（6）, c = 14.6818（9） A, α= 73.254（10）,β= 88.938（15）, γ= 68.080（10）°, V= 934.66（10） A3, Z = 2, F（000） = 400, Dc = 1.348 g/cm^3 and p = 0.094 mm-1. The final R = 0.0680 and wR = 0.1419 for 2142 observed reflections with I 〉 2σ（/）, and R = 0.1084 and wR = 0.1643 for all reflections. Two aromatic ring planes （pyrrole and phenanthroline rings） are connected by the amide plane. Two different types of intermolecular hydrogen bonds, O-H…N and N-H…O, exist in the crystal. The title complex molecules are connected through hydrogen bonds and weak π-π stacking interactions to generate a 3-D supramolecule.     

Ring-opened Crystal Structure and Photochromism of 2,2-Bis（4-tertiary butyl phenyl）-3H-naphtho[2,1-b]pyran

The title compound, 2,2-bis（4-tertial butyl phenyl） naphthopyran, has been prepared and characterized by means of IR, ^1H NMR and elemental analysis, and its crystal structure was determined with X-ray diffraction in the ring-opened form after hydrolyzation. It belongs to monoclinic, space group P21/c, with a = 14.358（3）, b = 7.6725（15）, c = 24.470（5） А, β= 97.147（4）°, C_33H_36O2, Mr=464.62, V= 2674.8（9）А^3, Z = 4, Dc = 1.154 g/cm^3,μ= 0.070 mm^-1, F（000） = 1000, the final R = 0.0514 and wR = 0.1272 for 5444 observed reflections （I 〉 2σ（I））. X-ray analysis revealed that the C（13）-O（1） bond of the title compound cracks after UV irradiation, the six-membered heterocycles are destroyed, and zwitterionic intermediates come into being. The molecular structure in the ring-opened form is obtained after hydrolyzation. It is infrequent that the single-crystal structure is determined in a ring-opened form. A two-dimensional framework is formed by O-H…O and CAr-H…O hydrogen bonds. The UV-vis spectra show that the title compound exhibits excellent photochromic properties in solutions and polymers.     

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

The title compound {[Zn（NIT4Py）（fum）（HEO）2]·H2O}n, where NIT4Py = 2-（4＇- pyridinyl）-4,4,5,5-tetra-methylimidazoline-looxyl-3-oxide and fum = 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, α= 94.608（2）, β = 92.328（2）, γ = 105.840（2）°, C16H24N3O9Zn, Mr = 467.75, V = 994.8（2） A^3, Z = 2, Dc = 1.562 g/cm^3,μ（MoKα） = 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 and Crystal Structure of a Co（ Ⅱ ） Complex with Taurine-5-methyl-2-hydroxyisophthalaldehyde Schiff Bases [Co（C13H16N2O7S2）（H2O）3]2·H2O

The title complex [CoL（H20）3]2·H2O （C26H46N4O21S4CO2）, where L = taurine-5- methyl-2-hydroxyisophthalaldehydes, has been synthesized and characterized by IR and X-ray diffraction analysis. The crystal of the complex belongs to the triclinic system, space group P1, with a = 11.197（4）, b = 13.309（5）, c = 14.486（5） ]A, a = 78.827（13）,β = 70.547（11）, γ = 81.058（13）°, Mr = 996.77, S = 1.08, V= 1987.2（13） A3, Z = 2, Dc = 1.666 g/cm3, F（000） = 1032,μ = 1.131 mm^-1, R = 0.0633 and wR = 0.1293. According to the structural analysis, the Co（ Ⅱ ） ion adopts a slightly distorted six-coordinated octahedral geometry. One N atom of the Schiff base of each molecule was hydrogenated to form hydrogen bond with O atom. Two coterminous molecules packed in one crystal water molecule are linked by intermolecular hydrogen bonds, thus generating an infinite chain constructed by hydrogen bonds.     

Synthesis,Crystal Structure and Theoretical Calculation of [2-（2,6-Dioxacyclohexyl）-5-methoxylphenols]2

The title compound [2-（2,6-dioxacyclohexyl）-5-methoxylphenols]2 was synthesized by the reaction of 2-hydroxyl-3-methoxylbenzaldehyde and 1,3-propanediol in the presence of DMF-DMS adduct and characterized by IR spectrum, UV-Vis spectrum and X-ray crystallography. The title compound belongs to monoclinic, space group P21 with a = 9.8967（10）, b = 8.2240（9）, c = 13.3654（14） A^°, β= 90.016（2）°, C11H14O4, Mr = 210.22, V = 1087.8（2）A^°3, Z = 4, Dc = 1.284 Mg/m^3, F（000） = 448,μ = 0.098 mm^-1, the final R = 0.0300 and wR = 0.0761 for 2070 observed reflections with I 〉 2σ（I）. The molecules are connected via intermolecular O-H…O hydrogen bonds into a 2D network structure. Moreover, theoretical investigations of the title compound with HF/6-31G（d） method were performed, and its stability, frontier molecular orbital composition and Mulliken charge distribution were also discussed. The compound is a bis-molecule. The two molecules stay together and could not be separated. Two crystallographically independent molecules exist in an asymmetric unit. The bond lengths and bond angles of the two molecules are slightly different with each other.     

Isolation and Crystal Structure of 4β,6α,9α- Trimethy-2-carboxyltricyclo[6.3.0.0^（4,5）]undec-2-ene

The title compound, 4β,6α,9α-trimethy-2-carboxyltricyclo[6.3.0.0^（4,5）]undec-2-ene, is a sesquiterpene which was first isolated from Ligularia caloxantha and characterized by MS and NMR. In addition, the structure was determined by X-ray single-crystal diffraction. It crystallizes in orthorhombie, space group P212121 with a = 8.197（2）, b = 14.876（3）, c = 22.281（6） A, α = β = γ = 90°, V = 2716.9（11） ]A^3, Z = 8, C15H22O2, Mr = 234.34, Dc = 1.146 g/cm^3, μ（MoKa） = 0.074 mm^-1, F（000） = 1024, the final R = 0.0384 and wR = 0.0856 for 6200 independent reflections （Rint = 0.066） and 2538 observed ones （I 〉 2σ（I））. In the molecule, there are three fused five-membered rings; while in this crystal form, the asymmetric unit contains two molecules of the same hand and they are linked together by two intermolecular O-H...O hydrogen bonds to form a dimer.     

Synthesis and Crystal Structure of Trans-4-[ （5-（ 2,4-Dichlorophenoxy）-3-methyl-1-phenyl-1H-pyrazol-4-yl）methyleneamino]-1,5-dimethyl-2-phenyl-l,2-dihydropyrazol-3-one

The title compound trans-4-[（5-（2,4-dichlorophenoxy）-3-methyl- 1-phenyl-1H-pyrazol-4-yl）methyleneamino]- 1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one 3 （C28H23Cl2N5O2, Mr = 532.41） has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in triclinic, space group P1- with a = 8.9438（4）, b = 11.6065（5）, c = 14.2215（6）A, α = 112.566（1）, β = 92.324（2）, γ = 102.91（1）°, V= 1315.65（10） A^3, Z = 2, Dc = 1.344 g/cm^3,μ（MoKa） = 0.282 mm^-1, λ = 0.71073 A, F（000） = 552, the final R = 0.0587 and wR = 0.1578 for 5071 observed reflections （I 〉 2σ（I））. X-ray analysis reveals that the product is a thermodynamically stable trans isomer. Intra- and intermolecular C（ 12）-H（12）…O（1） and C（28）-H（28）...O（1）# 1 hydrogen bonds were observed in the title compound.     

Synthesis,Crystal Structure and Antifungal Activity of N-（Pyridine-2-methyl）-2-（4- chlorophenyl）-3-methylbutanamide

A novel compound N-（pyridine-2-methyl）-2-（4-chlorophenyl）-3-methylbutanamide, a racemic compound, has been synthesized with 2-（4-chlorophenyl）-3-methylbutyric acid and pyridin- 2-methylanamine as the raw materials, and its crystal structure （C17H19C1N2O, Mr = 302.79） was determined by single-crystal X-ray diffraction analysis. The crystal belongs to monoclinic, space group P21/n with a = 9.624（9）, b = 23.14（2）, c = 15.626（15）A, β = 106.199（14）°, V = 3342（5） A^3, Z = 8, Dc = 1.204 g/cm^3,μ = 0.23 mm^-1, F（000） = 1280, S = 1.032, R = 0.0681 and wR = 0.1508 for 6513 unique reflections （Rint = 0.0421） with 3375 observed ones. In the crystal structure, there are some intermolecular hydrogen bonds which stabilize the crystal structure. The preliminary bioassay shows that the title compound exhibits good antifungal activity against Botrytis cinerea, Gibberella zeae, Dothiorella gregaria and Colletotrichum gossypii.