A dimeric luminescent lanthanide complex [Eu(PAA)2(phen)(NO3)]2: hydrothermal synthesis,crystal structure and fluorescence

A lanthanide coordination complex [Eu(PAA)₂(phen)(NO₃)]₂ (PAA?=?phenylacetic acid, phen?=?1,10-phenanthroline) has been synthesized by the hydrothermal method. Single crystal X-ray diffractions show that it forms a dimeric molecular structure. The title complex crystallizes in the triclinic system, space group P 1, with lattice parameters a?=?8.9473(8)?Å, b?=?13.3659(12)?Å, c?=?13.4745(12)?Å, α?=?60.7590(10)°, β?=?89.5100(10)°, γ?=?71.9850(10)°, V?=?1317.3(2)?ų, D _c?= 1.675?Mg?m^?3, Z?=?1, F(000)?=?660, GOF?=?1.003, R ₁?=?0.0206, wR ₂?=?0.0575. The fluorescence excitation and emission spectra have been investigated.     

A 1D coordination polymer {Pb[C6H4(COO)2][phen]} n with strong blue fluorescent emission

The hydrothermal reaction of 1,3-dicyanobenzene, 1,10-phenanthroline (phen) and Pb(CH₃COO)₂ yields a new 1D coordination polymer, {Pb[C₆H₄(COO)₂][phen]} _n . The 1,3-benzenecarboxylate anion found in the final product was generated in situ during the synthesis by hydrolysis of 1,3-dicyanobenzene. X-ray diffraction shows that complex 1 crystallizes in the triclinic system, space group P 1, a?=?7.5442(2)?Å, b?=?9.7962(3)?Å, c?=?13.1505(4)?Å, α?=?69.739(2)?Å, β?=?80.597(2)?Å, γ?=?71.377(2)?Å, v?=?862.48(4)?ų, Z?=?2, D _c?=?2.124 Mg?m^?3. Complex 1 emits strong blue fluorescent light (λem(max)?=?482.4?nm) when excited by UV light in the solid state at room temperature.     

Syntheses,crystal structures,and antimicrobial activities of nickel(II) and cadmium(II) complexes with 4-methylsulfonyl cinnamate and diamines

Two metal complexes, [Ni^II(mscinn)₂(pda)₂] (1) and [Cd^II(mscinn)₂(dmeda)₂·2H₂O] (2) (mscinn?=?4-methylsulfonyl cinnamate, pda?=?propane-1,3-diamine, dmeda?=?N′,N′-dimethylethane-1,2-diamine), were synthesized by reacting 4-methylsulfonyl cinnamate with the diamines and metal salts. Their structures were determined by single-crystal X-ray diffraction analysis. Crystal parameters of 1: C₂₆H₃₈N₄NiO₈S₂, M?=?657.43, monoclinic, P2₁/c, a?=?16.6123(8)?Å, b?=?8.5956(4)?Å, c?=?11.2047(5)?Å, β?=?107.423(1)°, V?=?1526.54(12)?ų, Z?=?2, D _calcd?=?1.430?g?cm^?3, F(000)?=?692, μ?=?0.825?mm^?1, R ₁?=?0.0257, wR ₂?=?0.0669. Crystal data of 2: C₂₈H₄₂CdN₄O₈S_2?·?2(H₂O), M?=?775.24, monoclinic, P2₁/c, a?=?9.8278(4)?Å, b?=?11.6611(5)?Å, c?=?15.3972(7)?Å, β?=?96.195(1)°, V?=?1754.26(13)?ų, Z?=?2, D _calcd?=?1.468?g?cm^?3, F(000)?=?804, μ?=?0.798?mm^?1, R ₁?=?0.0299, wR ₂?=?0.0770. Antimicrobial activities for 1 and 2 against Escherichia coli, Pseudomonas putida, Bacillus subtilis, and Bacillus cereus had better antibacterial activity than their parent carboxylic acid against Gram-positive bacteria (B. subtilis and B. cereus). The cadmium complex of the cinnamate displayed high inhibitory activity with an MIC value of 5?µg?mL^?1 against P. putida, while the nickel complex also exhibited good inhibitory potency with an MIC value of 5?µg?mL^?1 against B. subtilis.     

Rheological phase synthesis,characterization and magnetic property of a cobalt(II)diphosphonate

A new Co(II) diphosphonate compound, [Co(HEDPH₂)₂] (4,4′-bipyH₂)?·?H₂O (1) has been successfully obtained by a rheological phase reaction at 80°C. Single-crystal diffraction analysis shows a 1-D chain structure and the 1-D chains are assembled via hydrogen bonds into a 3-D supramolecular structure with channels. The protonated 4,4′-bipy molecules are encapsulated in the channels. Magnetic study shows 1 to exhibit antiferromagnetic interaction in the 1D Co--O--P--O--Co chain. Crystal data for 1: monoclinic, space group Cc, a?=?15.754(6)?Å, b?=?14.457(5)?Å, c?=?10.020(4)?Å, β?=?92.024(6)°, V?=?2280.7(14)?ų, Z?=?4.     

Synthesis,structure and characterization of copper(II) and zinc(II) complexes based on 3-carboxyl-1,2,4-triazole

Two complexes [CuL₂(H₂O)₂] (1) and [ZnL₂(H₂O)₂] (2) (L?=?3-carboxyl-1,2,4-triazole (L)) have been synthesized and characterized by single-crystal X-ray diffraction analysis. Compound 1 crystallizes in the monoclinic space group P ₂(1)/n, a?=?8.632(8)?Å, b?=?9.153(8)?Å, c?=?6.991(7)?Å, β?=?94.279(12)°, Z?=?2, R ₁?=?0.0296, wR ₂?=?0.0918. Compound 2 also crystallizes in the monoclinic space group P ₂(1)/n, a?=?4.937(3)?Å, b?=?18.107(10)?Å, c?=?6.344(4)?Å, β?=?106.839(7)°, Z?=?2, R ₁?=?0.0230, wR ₂?=?0.0556. Extensive intermolecular hydrogen bonds assemble 1 and 2 into three-dimensional (3D) supramolecular architectures, with eight-member H-bonded synthons. Compounds 1 and 2 were also characterized by element analysis, FT–IR, luminescence and EPR studies.     

Hydrothermal synthesis,structures and characterization of two new copper(II) triphosphonate compounds

Two copper(II) triphosphonate compounds, Cu[(APTPH₄)(phen)(H₂O)]?·?2.16H₂O (1) and [Cu(APTPH₄)(2,2′-bipy)(H₂O)]?·?2.63H₂O (2), have been prepared by a low temperature hydrothermal reaction from 1-aminopropane-1,1,3-triphosphonic acid (APTPH₆), CuO and a second ligand, phen?=?1,10-phenanthroline, or 2,2′-bipy?=?2,2′-bipyridyl. These two compounds were characterized by single crystal X-ray diffraction, elemental analysis, IR and TG. Crystal data for 1: Monoclinic, space group P2₁ /c, a?=?14.4830(7)?Å, b?=?9.1721(5)?Å, c?=?16.7403(8)?Å, β?=?90.101(2)°. For compound 2: Triclinic, space group P 1, a?=?7.1215(7)?Å, b?=?10.460(2)?Å, c?=?14.671(2)?Å, α?=?82.983(2)°, β?=?83.882(2)°, γ?=?80.617(2)°. In both compounds, each Cu²⁺ ion is five-coordinate with two oxygen atoms from the triphosphonate, two nitrogen atoms from the second ligand and one water molecule, to form a distorted square-pyramidal geometry. Both complexes have 3D supramolecular structures constructed by hydrogen bonds and π–π stacking interactions.     

Synthesis and characterization of a dinuclear (Hedta)Ru(III) complex

A ruthenium(III) complex containing ethylenediaminetetraacetate (edta), [{Ru(Hedta)}₂(Pyz)]?·?8H₂O (1) (Pyz?=?pyrazine), has been synthesized by the reaction between K[Ru(Hedta)Cl]?·?1.5H₂O and pyrazine. The structure of the complex was determined by single X-ray diffraction. Complex 1 crystallizes in the triclinic space group P 1 with a?=?7.293(9)?Å, b?=?10.575(14)?Å, c?=?12.742(16)?Å, α?=?104.044(19)°, β?=?91.893(19)°, γ?=?93.35(2)°, Z?=?1. The product was also characterized by IR, UV-Vis, EPR spectrum and magnetic techniques.     

Syntheses,structural determination,and binding studies of nine-coordinate mononuclear (mnH)2[DyIII(Httha)]·3H2O and (enH2)3[DyIII(ttha)]2·9H2O

Two dysprosium coordination compounds, (mnH)₂[Dy^III(Httha)]·3H₂O (1) (H₆ttha?=?triethylenetetramine-N,N,N′,N″,N′′′,N′′′-hexaacetic acid and mn?=?methylamine) and (enH₂)₃[Dy^III(ttha)]₂·9H₂O (2) (en?=?ethylenediamine), were synthesized through direct heating and characterized by elemental analysis, FT-IR, thermal analysis, and single-crystal X-ray diffraction. X-ray diffraction analysis displays that 1 is a mononuclear nine-coordinate complex with a pseudo-monocapped square antiprismatic conformation (MCSAP) crystallizing in the monoclinic crystal system with P2(1)/c space group. The crystal data are as follows: a?=?16.1363(19)?Å, b?=?13.9336(11)?Å, c?=?13.6619(14)?Å, β?=?102.2490(10)°, and V?=?3001.8(5)?ų. There are two kinds of methylamine cation in 1. They connect [Dy^III(Httha)]^2?and crystal waters through hydrogen bonds, leading to formation of a 2-D ladder-like layer structure. The polymeric 2 also is a nine-coordinate structure with a pseudo-MCSAP crystallizing in the monoclinic crystal system with P2/c space group. The cell dimensions are: a?=?17.7801(16)?Å, b?=?9.7035(10)?Å, c?=?22.096(2)?Å, β?=?118.874(2)°, and V?=?3338.3(6)?ų. In 2 there are also two types of ethylenediamine cations. One connects three adjacent [Dy^III(ttha)]^3? complex anions through hydrogen bonds and the other is symmetrical forming hydrogen bonds with two neighboring [Dy^III(ttha)]^3? complex anions. These hydrogen bonds result in formation of a 2-D ladder-like layer structure as well.     

Synthesis and crystal structure of a Cu(II) complex with mixed malonate/1,10-phenanthroline ligands

A Cu(II) complex with mixed ligands, [Cu₃(mal)₃(phen)₃(H₂O)₂]?·?11H₂O (mal?=?malonate, phen?=?1,10-phenanthroline) was synthesized and characterized by elemental analysis, IR, UV, electron paramagnetic resonance (EPR) and luminescence spectra and single-crystal X-ray diffraction. The complex crystallizes in the monoclinic system, space group Cc with a?=?13.1631(10)?Å, b?=?20.1089(10)?Å, c?=?20.1267(13)?Å, β?=?103.500(3)°, V?=?5180.2(6)?ų, Z?=?4, and R ₁?=?0.0476 for 7993 observed reflections. In the complex, one Cu is coordinated by a mal dianion and a phen molecule, exhibiting N₂O₂ square-planar geometry, while the other two Cu atoms are coordinated, respectively, by a mal dianion, a phen and water molecules, exhibiting N₂O₃ square pyramidal coordination geometry.     

Syntheses and structural determinations of the nine-coordinate rare earth metal: Na4[DyIII(dtpa)(H2O)]2·16H2O,Na[DyIII(edta)(H2O)3]·3.25H2O and Na3[DyIII(nta)2(H2O)]·5.5H2O

Three complexes, Na₄[Dy^III(dtpa)(H₂O)]₂?·?16H₂O, Na[Dy^III(edta)(H₂O)₃]?·?3.25H₂O and Na₃[Dy^III (nta)₂(H₂O)]?·?5.5H₂O, have been synthesized in aqueous solution and characterized by FT–IR, elemental analyses, TG–DTA and single-crystal X-ray diffraction. Na₄[Dy^III(dtpa)(H₂O)]₂?·?16H₂O crystallizes in the monoclinic system with P2₁/n space group, a?=?18.158(10)?Å, b?=?14.968(9)?Å, c?=?20.769(12)?Å, β?=?108.552(9)°, V?=?5351(5)?ų, Z?=?4, M?=?1517.87?g?mol^?1, D _c?=?1.879?g?cm^?3, μ?=?2.914?mm^?1, F(000)?=?3032, and its structure is refined to R ₁(F)?=?0.0500 for 9384 observed reflections [I?>?2σ(I)]. Na[Dy^III(edta)(H₂O)₃]?·?3.25H₂O crystallizes in the orthorhombic system with Fdd2 space group, a?=?19.338(7)?Å, b?=?35.378(13)?Å, c?=?12.137(5)?Å, β?=?90°, V?=?8303(5)?ų, Z?=?16, M?=?586.31?g?mol^?1, D _c?=?1.876?g?cm^?3, μ?=?3.690?mm^?1, F(000)?=?4632, and its structure is refined to R ₁(F)?=?0.0307 for 4027 observed reflections [I?>?2σ(I)]. Na₃[Dy^III(nta)₂(H₂O)]?·?5.5H₂O crystallizes in the orthorhombic system with Pccn space group, a?=?15.964(12)?Å, b?=?19.665(15)?Å, c?=?14.552(11)?Å, β?=?90°, V?=?4568(6)?ų, Z?=?8, M?=?724.81?g?mol^?1, D _c?=?2.102?g?cm^?3, μ?=?3.422?mm^?1, F(000)?=?2848, and its structure is refined to R ₁(F)?=?0.0449 for 4033 observed reflections [I?>?2?σ(I)]. The coordination polyhedra are tricapped trigonal prism for Na₄[Dy^III(dtpa)(H₂O)]₂?·?16H₂O and Na₃[Dy^III(nta)₂(H₂O)]?·?5.5H₂O, but monocapped square antiprism for Na[Dy^III(edta)(H₂O)₃]?·?3.25H₂O. The crystal structures of these three complexes are completely different from one another. The three-dimensional geometries of three polymers are 3-D layer-shaped structure for Na₄[Dy^III(dtpa)(H₂O)]₂?·?16H₂O, 1-D zigzag type structure for Na[Dy^III(edta)(H₂O)₃]?·?3.25H₂O and a 2-D parallelogram for Na₃[Dy^III(nta)₂(H₂O)]?·?5.5H₂O. According to thermal analyses, the collapsing temperatures are 356°C for Na₄[Dy^III(dtpa)(H₂O)]₂?·?16H₂O, 371°C for Na[Dy^III(edta)(H₂O)₃]?·?3.25H₂O and 387°C for Na₃[Dy^III(nta)₂(H₂O)]?·?5.5H₂O, which indicates that their crystal structures are very stable.     

Synthesis and structures of two cobalt complexes [NaCoII(NTA)(H2O)] n and NH4[CoIII(IDA)2] · 2H2O

Two cobalt complexes [NaCo^II(nta)(H₂O)] _n (H₃nta?=?nitrilotriacetic acid) (1) and NH₄[Co^III(ida)₂]?·?2H₂O (H₂ida?=?iminodiacetic acid) (2) have been synthesized and characterized by single-crystal X-ray diffraction analysis. Compound 1 crystallizes in the orthorhombic system, space group P2₁2₁2₁ with a?=?7.9770(12)?Å, b?=?9.7613(15)?Å, c?=?12.1945(18)?Å, V?=?949.5(2)?ų, Z?=?4, and R ₁?=?0.0705 for 1597 observed reflections. Compound 2 crystallizes in the monoclinic system, space group P2(1)/c with a?=?5.1801(3)?Å, b?=?11.2073(6)?Å, c?=?12.2891(7)?Å, V?=?707.09(7)?ų, Z?=?2, and R ₁?=?0.0349 for 1143 observed reflections. In compound 1, the Co is coordinated by a nitrogen and five oxygen atoms in a distorted octahedral geometry {CoNO₅}, and the Na is coordinated by one water molecule and four carboxyl oxygen atoms in slightly distorted square pyramidal geometry. The entire structure shows a three-dimensional network. In compound 2, Co atom is equatorially coordinated by two ida ligands in a distorted octahedral geometry {CoN₂O₄}. The discrete [Co(ida)₂]^2? anions are linked by hydrogen bonding to a three-dimensional supramolecular network.     

Syntheses,crystal structures,and fluorescence properties of two isomorphic binuclear compounds incorporating N-acetyl-N-phenylglycinate with N-donor co-ligands

In this study, two new isomorphic binuclear compounds, [Ln(µ-NAP)₄(NAP)₂(phen)₂]?·?H₂O (1) and (2) (Ln?=?Eu, Tb, NAP?=?N-acetyl-N-phenylglycinate; phen?=?1,10-phenanthroline), have been synthesized and characterized by infrared spectroscopy, elemental analysis, and X-ray crystallography. These compounds crystallize in a triclinic form with space group Pī with a?=?11.7519(11), b?=?13.4293(12), c?=?14.0686(13)?Å, V?=?1992.7(3)?ų, and Z?=?1. Single-crystal X-ray structural analysis reveals that 1 is binuclear, assembled into a 3-D supramolecular network with self-complementary double hydrogen-bonding interactions and aromatic π–π interactions. Fluorescence properties of 1 and 2 are also discussed.     

Hydrothermal synthesis and characterization of two new arsenic–vanadate compounds with the same cluster anion [As8V14O42(H2O)]4−

Two new arsenic–vanadate compounds [Co(C₄H₁₃N₃)₂]₂[As₈V₁₄O₄₂(H₂O)]?·?3.5H₂O (1) and (C₂N₂H₉)₂(C₂N₂H₁₀)[As₈V₁₄O₄₂(H₂O)]?·?2.33H₂O (2) have been hydrothermally synthesized and characterized by X-ray single crystal diffraction, IR spectra and thermogravimetric analysis. Compound 1 crystallizes in the monoclinic space group P ₂(1)/c, a?=?24.649(9)?Å, b?=?13.364(5)?Å, c?=?22.463(8)?Å, β?=?104.008(5)°, V?=?7180(5)?ų, Z?=?4, R ₁?=?0.0787, and wR ₂?=?0.1859. Compound 2 crystallizes in rhombohedral system with space group R3c, a?=?b?=?c?=?22.2405(5)?Å, α?=?β?=?γ?=?110.4030(10)°, V?=?8163.4(3)?ų, Z?=?6, R ₁?=?0.0341 and wR ₂?=?0.0941. The structural analyses show that both compounds have the same discrete cluster anion [As₈V₁₄O₄₂(H₂O)]^4?. Moreover, in 1, the polyanions are connected through van der Waals forces to generate soft channels that are filled by [Co(C₄H₁₃N₃)₂]²⁺ cations and water. In 2, water and organic molecules link cluster anions to create the supramolecular assembly through hydrogen bonding.     

Syntheses,crystal structures and magnetic study of two binuclear manganese(II) complexes with aromatic N-oxide as bridging ligand

Two new binuclear complexes, [Mn₂(μ-dmpo)₂(SCN)₄(H₂O)₂] (1) (where dmpo?=?3,5-dimethylpyridine N-oxide), [Mn₂(μ-po)₂(H₂O)₆I₂]I₂ (2) (where po?=?pyridine N-oxide), have been synthesized and their crystal structures determined by X-ray crystallography. Complexes 1 and 2 crystallize in monoclinic, space group P2₁/c, with unit cell dimensions a?=?8.8836(18)?Å, b?=?15.450(3)?Å, c?=?15.484(3)?Å, β?=?91.020(3)° for 1, and a?=?8.8352(13)?Å, b?=?17.927(3)?Å, c?=?8.3338(12)?Å, β?=?103.765(2)° for 2. In each binuclear complex two Mn(II) were bridged by two 3,5-dimethylpyridine N-oxides or by two pyridine N-oxides and the distances between the bridged Mn(II) ions are 3.599?Å for 1 and 3.552?Å for 2. Variable temperature (4–300?K) magnetic measurements were performed for 1 and the susceptibility data were fitted by using a binuclear Mn(II) magnetic coupling formula producing the 2J?=??2.17?cm^?1.     

Synthesis and structures of three triphosphonate compounds containing d10 transition metal ions

Three new triphosphonate compounds, [Zn(APTPH₄)(2,2′-bipy)(H₂O)]?·?2H₂O (1), [Cd(APTPH₄)(2,2′-bipy)(H₂O)]?·?2H₂O (2), and [Zn(APTPH₄)(phen)₂]?·?phen?·?4H₂O (3) (APTPH₆?=?1-aminopropane-1,1,3-triphosphonic acid, 2,2′-bipy?=?2,2′-bipyridine, phen?=?1,10-phenanthroline), are synthesized by a low-temperature hydrothermal method. Compounds 1 and 2 are isomorphous, both one-dimensional (1D) coordination polymers expanded into three-dimensional (3D) supramolecular structures by hydrogen bonds and π–π stacking interactions. Compound 3 is a molecular complex and forms a 3D network through an S-shaped water hexamer. Crystal data for 1: Triclinic, space group P 1, a?=?6.6814(5)?Å, b?=?10.0929(7)?Å, c?=?15.438(2)?Å, α?=?81.544(2)°, β?=?79.066(2)°, γ?=?82.278(2)°, Z?=?2; for 2: Triclinic, space group P 1, a?=?6.9380(8)?Å, b?= 10.043(2)?Å, c?=?15.681(2)?Å, α?=?81.357(2)°, β?=?78.510(2)°, γ?=?81.902(2)°, Z?=?2; Crystal data for 3: Triclinic, space group P 1, a?=?12.540(2)?Å, b?=?12.596(2)?Å, c?=?14.997(2)?Å, α?=?100.795(2)°, β?=?113.328(2)°, γ?=?101.358(2)°, Z?=?2.     

Synthesis,structure, and DNA-binding studies of a dicopper(II) complex with N-phenolato-N′-[2-(dimethylamino) ethyl]oxamide as ligand

A new µ-oxamido-bridged dicopper(II) complex, [Cu₂(pdmaeox)(bpy)(H₂O)](pic)?·?H₂O [H₃pdmaeox?=?N-phenolato-N′-[2-(dimethylamino)ethyl]oxamide, Hpic?=?2,4,6-trinitrophenol, bpy?=?2,2′-bipyridine], has been synthesized and characterized by elemental analyses, molar conductivity measurement, infrared, and electronic spectra studies, and X-ray single-crystal diffraction. The complex crystallizes in the triclinic system, P 1 space group, with crystallographic data: a?=?10.7815(2)?Å, b?=?11.3598(2)?Å, c?=?14.1389(3)?Å, and z?=?2. In [Cu₂(pdmaeox)(bpy)(H₂O)]⁺, one copper(II) resides in the inner site with a square-planar coordination geometry and the other is chelated by the two exo-oxygen atoms of the cis-pdmaeox^3? ligand in a square-pyramidal environment. The Cu···Cu separation through cis-pdmaeox^3? bridge is 5.1834(4)?Å. The crystal structure is stabilized by hydrogen bonds and π–π stacking interactions. The interaction of the dicopper(II) complex with herring sperm-DNA (HS-DNA) has been investigated by electronic absorption titration, fluorescence titration, electrochemical titration, and viscosity measurements. The results reveal that the interaction of the dicopper(II) complex with HS-DNA might be electrostatic binding. The effects of bridging ligand on the interaction of the dinuclear complex with HS-DNA were preliminarily investigated.     

Hydrothermal syntheses,crystal structures,and thermal stability of two new 3D open-framework metal(II) phosphonates

This article reports the hydrothermal synthesis and characterization of two new phosphonate compounds NaCo[O₃PCH(OH)CO₂] (1) and NaMn[O₃PCH(OH)CO₂] (2) based on 2-hydroxyphosphonoacetic acid (H₃L). Their structures have been characterized by single-crystal X-ray diffraction as well as with elemental analysis, infrared spectroscopy and thermogravimetric analysis. The two isomorphous compounds crystalline in the orthorhombic, space group Pbca: Crystal data for 1: a?=?10.1827(8)?Å, b?=?9.6673(8)?Å, c?=?10.7853(9)?Å, V?=?1061.70(15)?ų, Z?=?8, R ₁?=?0.0252, wR ₂?=?0.0577; Crystal data for 2: a?=?10.4309(18)?Å, b?=?9.7913(17)?Å, c?=?10.9012(19)?Å, V?=?1113.4(3)?ų, Z?=?8, R ₁?=?0.0194, wR ₂?=?0.0536. In the two compounds, the metal atoms are octahedrally coordinated; all oxygen atoms from the H₃L ligand are involved in coordination. The overall structures can be described as a 3D open framework with channels running along the a axis and the charge-compensating Na⁺ cations being located at the intersections of these channels.     

Synthesis,structure and magnetic properties of Ni2(NO3)4(APTY)4 (APTY=1,5-dimethyl-2-phenyl-4-{[(1 E )-pyridine-4-ylmethylene]amino}-1,2-dihydro-3 H -pyrazol-3-one)

A novel dinuclear nickel(II) complex Ni₂(NO₃)₄(APTY)₄ (1) (APTY?=?1,5-dimethyl-2-phenyl-4-{[(1E)-pyridine-4-ylmethylene]amino}-1,2-dihydro-3H-pyrazol-3-one), was synthesized by solvothermal reaction of Ni(NO₃)₂?·?6H₂O with APTY in methanol at 353?K. The structure consists of centrosymmetric dimers resulting from octahedrally coordinated Ni atoms bridged by APTY ligands. Weak intermolecular interactions (C–H?···?N, C–H?···?O hydrogen bonding, C–H?···?π and π–π stacking interactions) are responsible for a supramolecular assembly of molecules in the lattice. Magnetic measurements over 1.8–300?K show weak antiferromagnetic coupling between Ni(II) ions with J?=?2.969?cm^?1, g?=?2.280, θ?=??5.903.     

Hydrothermal synthesis and crystal structure of a layered coordination polymer: [Zn2(C2O4)2(C3N2H4)2] n

A new metal-organic coordination polymer [Zn₂(C₂O₄)₂(C₃N₂H₄)₂] _n (1) has been hydrothermally synthesized with ZnCl₂·2H₂O, oxalic acid and imidazole. The compound has a 2D network, consisting of infinite zinc(II) oxalate chains connected to each other by three-coordinate oxygen atoms. Within the chains, the zinc atoms are each octahedrally coordinated by one nitrogen atom from imidazole and five oxygen atoms from oxalate groups. Furthermore, there are two coordination modes of oxalate to zinc ions: chelate bis-bidentate and chelate/bridging bis-bidentate in compound 1, and the latter is rare among related compounds. Crystal data: monoclinic, P2(1)/c, a?=?8.4310(17), b?=?9.4060(19), c?=?8.2790(17)?Å, β?=?93.15(3)°, V?=?655.5(2)?ų, Z?=?2, R ₁?=?0.0322, wR ₂?=?0.0850.