Yue Zhuang

Synthesis and crystal structures of supramolecular compounds: [Cu(mpca)2(H2O)] · 3H2O and [Cu2(mpca)2(pyr)4]

A new chelate ligand, 5-methyl-1H-pyrazole-3-carboxylic acid (mpca), has been synthesized. This ligand reacts with cupric sulfate to give two supramolecular compounds [Cu(mpca)2(H2O)] · 3H2O (1) and [Cu2(mpca)2(pyr)4] (Pyr = pyridine) (2), which were characterized by elemental analysis and X-ray crystal diffraction. Helical water chain and strong π–π interaction are important for the stability of the 3-D structure of these supramolecules.

Diaqua-bis(1H-1,2,4-triazole-3-carboxyl-ato)cadmium(II).

In the title complex, [Cd(C3H2N3O2)2(H2O)2], the CdII atom is coordinated by two N and two O atoms from two deprotonated 1H-1,2,4-triazole-3-carboxylic acid ligands (TRIA) and two water molecules. The Cd atom is located on an inversion centre. In the crystal structure, molecules are linked together via O—H⋯O and N—H⋯O hydrogen bonds, forming a three-dimensional network.

Synthesis, Structure, Thermal and Fluorescent Properties of a Novel Mn(II) Coordination Polymer and its Hexacyclic Water Ring

A novel Imazethapyr-bridged complex [Mn(Ima)2] (H2O)2 (1) [Imazethapyr (Ima)=5-ethyl-2-(5-isopropyl-5-methyl-4-oxo-4,5-dihydro-1H-imidazol-2-yl) nicotinic acid, has been synthesized and structurally characterized by X-ray diffraction method, infrared spectra, elemental analysis and thermal analysis. The title polymer contains a monocyclic hexamer water cluster, and the cluster plays an important role in stabilizing the complex. The fluorescence of the complex 1 in the solid state was investigated via FL55 spectrophotometer and it indicated a fluorescent behavior at room temperature.Graphical AbstractA novel Imazethapyr-bridged complex [Mn(Ima)2] (H2O)2 [Imazethapyr (Ima) = 5-ethyl-2-(5-isopropyl-5-methyl-4-oxo-4,5-dihydro -1H-imidazol-2-yl) nicotinic acid, has been synthesized and structurally characterized by X-ray diffraction method, infrared spectra, elemental analysis and thermal analysis. The title polymer contains a monocyclic hexamer water cluster, and the cluster plays an important role in stabilizing the complex.

3‐Chloro‐6‐(3,5‐dimethyl‐1H‐pyrazol‐1‐yl)picolinic acid

In the title compound, C11H10ClN3O2, the dihedral angle between the two rings is 5.6°. The crystal structure is stabilized by O—H⋯O hydrogen bonds.

Crystal structure of bis[2-(2,4-difluorophenyl)-1,3-bis(1,2,4-triazol-1-yl)propan-2-ol]-bis[5-ethyl-2-(4-isopropyl-4-methyl-5-oxo-2-imidazolin-2-yl)nicotinato]manganese(II), Mn(C13H12F2N6O)2(C15H18N3O3)2

C56H60F4MnN18O8, triclinic, P1 (no. 2), a = 9.7450(6) Å, b = 11.2747(6) Å, c = 15.2325(8) Å, + = 79.072(4)°, ) = 78.248(4)°, & = 65.073(3)°, V = 1475.7 Å, Z = 1, Rgt(F) = 0.048, wRref(F) = 0.139, T = 296 K. Source of material An ethanol solution of 2-(2,4-difluorophenyl)-1,3-bis(1,2,4triazol-1-yl)propan-2-ol (Fluconazole, HFlu, 0.05 mmol) and 5ethyl-2-(4-isopropyl-4-methyl-5-oxo-2-imidazolin-2-yl)nicotinic acid (Imazethapyr, Imaz, 0.05 mmol) were added to a solution of manganese chloride (0.2 mmol) in water (10 ml). Then a purple solution was obtained. The crystals were obtained by evaporating the solution at room temperature for several days. Elemental analysis — found: C, 53.79 %; H, 5.16 %; N, 20.26 %; calculated for C56H60F4MnN18O8: C, 53.84 %; H, 5.13 %; N, 20.19 %. Experimental details The isopropyl, methyl, N12 and O5 of the imidazole ring of the Imaz are disordered with occupancy of 0.5/0.5. Discussion 2-(2,4-Difluorophenyl)-1,3-bis(1,2,4-triazol-1-yl)propan-2-ol (HFlu) is one of the first-line popular drugs used to treat invasive infections [1]. 5-Ethyl-2-(4-isopropyl-4-methyl-5-oxo-2-imidazolin-2-yl)nicotinic acid (IMaz) is an imidazole compound used as a selective herbicide [2]. Both of them would be an interesting candidate to construct coordination polymers, since it combines the features required for coordination to metal ions through nitrogen atoms and oxygen atoms for extended intermolecular interactions. Thus, the HFlu and Imaz ligands are potential to construct a diversity of coordination architectures upon the metal complexation. The crystal structure of the title complex consists of divalent manganese cation coordinated by six N atoms. Two N atoms originate from two triazole of two different HFlu molecules and the other four N atoms are from two different imazethapyr anions (two N atoms from two pyridyl rings and the other two N atoms from two oxo-imidazole rings). The lengths of Ni—N bonds are in the range of 2.220(2) 2.304(1) Å. The associated angles range from 71.54(5)° to 180.00(5)°. It indicates that manganese(II) has a distorted octahedral coordination. The pyridinyl ring C2–C3–C4–C5–C6–N3 and the triazole ring N2–C17–N9– Z. Kristallogr. NCS 225 (2010) 213-215 / DOI 10.1524/ncrs.2010.0092 213

Bis[μ-2-(2,4-difluoro­phen­yl)-1,3-bis­(1H-1,2,4-triazol-1-yl)propan-2-olato]dicopper(II) bis­(perchlorate)

The title complex, [Cu2(C13H11F2N6O)2](ClO4)2, which was hydrothermally synthesized, contains a binuclear copper cluster (2 symmetry) with a Cu2O2 rhombus [Cu—O = 1.927 (2) Å] formed by donation of two O atoms from two chelate rings. The tridentate function of each ligand is completed by two N atoms coordinated to the two CuII atoms [Cu—N = 1.933 (2) Å]. The separation distance of two CuII atoms in a cluster is 2.988 (1) Å. The dihedral angle between the six-membered chelate rings is 2.13 (9)°. The perchlorate counter-anion is disordered over two sites in a 0.58 (10):0.42 (10) ratio.

catena-Poly[[[diaqua­sodium]-di-μ-aqua] 2-(2-pyrid­yl)quinoline-4-carboxyl­ate]

In the title compound, [Na(H2O)4](C15H9N2O2), the Na+ ion is coordinated by six water molecules in an octahedral geometry. The NaO6 octahedra are connected by sharing edges, forming a cationic chain along the b-axis direction. O—H⋯O and O—H⋯N hydrogen bonds link the chains and the 2-(2-pyridyl)quinoline-4-carboxylate anions into a two-dimensional network parallel to (100).

Bis[μ-2-(2,4-difluoro­phen­yl)-1,3-bis­(1,2,4-triazol-1-yl)propan-2-olato-κ4N2,O:O,N2′]bis­[(acetato-κ2O,O′)nickel(II)] methanol hemisolvate

In the title complex, [Ni2(C13H11F2N6O)2(C2H3O2)2]·0.5CH3OH, there are two half-molecules in the asymmetric unit. The two centrosymmetrically related NiII atoms, each attached to an acetate ligand, are linked by two fluconazole ligands. Each NiII atom is six-coordinated in a distorted octahedral geometry by two N atoms of the triazole groups and two bridging O atoms from two different fluconazole ligands and two O atoms from a chelating acetate ligand. In the crystal structure, the half-occupied methanol solvent molecule is linked to a triazole group via an O—H⋯N hydrogen bond.

Aqua­[2-(5-ethyl-2-pyridyl-κN)-4-iso­propyl-4-methyl-5-oxo-4,5-dihydroxy­imidazol-1-ido-κN1](5-methyl-1H-pyrazole-3-carboxyl­ato-κ2N2,O)copper(II) 1.33-hydrate

In the title complex, [Cu(C(5)H(5)N(2)O(2))(C(14)H(18)N(3)O)(H(2)O)]·1.33H(2)O, the Cu(II) ion is coordinated in a slightly distorted square-pyramidal environment. The basal plane is formed by two N atoms from a 2-(5-ethyl-2-pyridyl-κN)-4-isopropyl-4-methyl-5-oxo-4,5-dihydroxy-imidazol-1-ide ligand and by one O atom and one N atom from a 5-methyl-1H-pyrazole-3-carboxyl-ate ligand. The apical position is occupied by a water mol-ecule. In the crystal structure, O-H⋯O, O-H⋯N and N-H⋯O hydrogen bonds lead to a three-dimensional supra-molecular network.

3,6-Dichloro-N-(4,6-dichloro­pyrimidin-2-yl)picolinamide

In the title compound, C10H4Cl4N4O, the pyridine and pyrimidine rings are nearly perpendicular to each other, the dihedral angle between them being 86.60 (10)°. In the crystal structure, the N and O atoms in the amide group are involved in intermolecular hydrogen bonds, forming a one-dimensional chain along the c axis.