Synthesis and structure of a novel 3D Cd(II) supramolecule based on 2-propyl-imidazole-4,5-dicarboxylate

A novel supramolecule [Cd(H₂PIDC)2 · 2H₂O] · 3.5H₂O (I) (H₂PIDC^? = the deprotonated 2-propyl-imidazole-4,5-dicarboxylate) has been synthesized and characterized by X-ray diffraction method. Compound I crystallizes in the triclinic space group \(P\bar 1\) with cell parameters a = 10.6307(11) Å, b = 10.7068(12) Å, c = 11.3731(12) Å, α = 83.6470(10)°, β = 81.7310(10)°, γ = 87.3720(10)°, V = 1272.6(2) å³, Z = 2, ρ_calc = 1.581 g/cm³, F(000) = 618. It is a mononuclear complex consisting of a Cd(II) ion, two H₂PIDC-ligands and two coordinated water molecules, together with three and a half uncoordinated water molecules. The Cd(II) ion displays a slightly distorted octahedral geometry, defined by two N,O-bidentate H₂PIDC-ligands and two water molecules. Five-water clusters along with other intermolecular hydrogen bonds contribute to the construction of a three-dimensional supramolecular network.     

Hydrothermal synthesis and properties of a new 3D lanthanum supramolecule based on the 4-hydroxypyridine 2,6-dicarboxylate and water ligands

A hydrogen-induced lanthanum complex, (HDMA)⁺[La(HCAM)₂(H₂O)₃]^? · 2H₂O (I) (H₃CAM = 4-hydroxypyridine-2,6-dicarboxylic acid, DMA = dimethylamine), has been synthesized in a H₂O-DMF (DMF = dimethylformamide) mixed solution and characterized by elemental analysis, IR spectroscopy, and X-ray single-crystal diffraction. Complex I crystallizes in the triclinic system, space group P $ \bar 1 $ a = 10.2755(11), b = 10.4507(11), c = 12.0016(13) Å, α = 92.3510(10)°, β = 92.980(4)°, γ = 117.2670(10)°, V = 1143.4(2) ų, M _r = 637.29, ρ _c = 1.851 g/cm³, and Z = 2. The complex presents one-dimensional (ID) zigzag chain array, and these 1D chains are further linked into 3D supramolecular frameworks by extensive intra- and intermolecular hydrogen-bonding interactions. The luminescence emission spectra of the complex exhibits favorable fluorescent emission resulted from the ligand-to-metal electron transfer.     

Synthesis,crystal structure and magnetic properties of a new 3D coordination polymer constructed by Co(II) with pyridine-3,4-dicarboxylate and 4,4’-bipyridine

A metal-organic framework, [Co₂(pydc)₂(bpy)₂] _n · 2nH₂O (1) (H₂pydc = pyridine-3,4-dicarboxylic acid, bpy = 4,4′-bipyridine), was synthesized under hydrothermal conditions. X-ray diffraction experiments reveal that (1) exhibits a chiral 3D metal-organic framework, which represents the rare example of 3D chiral coordination polymers containing two kinds of organic ligands. Temperature-dependent magnetic susceptibility for (1) was also studied. Electronic Supplementary Material Supplementary material is available to authorised users in the online version of this article at .     

Synthesis, structure, and thermal stability of a new 2D copper(II) coordination polymer based on 2-propyl-1H-imidazole-4,5-dicarboxylate

A new Cu(II) coordination polymer with singly deprotonated 2-propyl-imidazole-4,5-dicarboxylate (H₃PIDC) as bridging ligand of formula [Cu(H₂PIDC)₂] _n (I) was synthesized and characterized by IR, element analysis, and X-ray diffraction method. Compound I crystallizes in the monoclinic space group P2₁/n with cell parameters a = 8.332(1), b = 10.160(1), c = 11.228(1) Å, β = 91.13(1)°, V = 950.3(2) ų, M _r = 457.88, Z = 2, ρ _c = 1.600 g/cm³, F(000) = 470, μ = 1.202 mm^?1, R ₁ = 0.0412, and wR ₂ = 0.1064 for 2015 observed reflections. The Cu²⁺ ions are coordinated by four H₂PIDC^? ligands via N,O-chelating and O-bridging mode to form 2D layer planes, which are further linked by intermolecular hydrogen bonds and weak interactions into a 3D framework.     

Solvothermal synthesis,crystal structure,and characterization of two new 2D Co(II)/Ni(II) coordination polymers with mixed-organic tectonics

Two new isomorphous coordination polymers [Co(4,4′-Bpda)(Dpa)] _n (I) and [Ni(4,4′-Bpda)(Dpa)] _n · H₂O (II) (4,4′-H₂Bpda = benzophenone-4,4′-dicarboxylic acid, Dpa = dipyridin-4-ylamine) were synthesized under solvothermal condition and characterized by elemental analysis, FT-IR and single-crystal X-ray diffraction technique. Compounds I and II exhibit 2D helical layers resulting from alternating single helical chains and double helical chains, which feature uninodal 4-connected topology with a point symbol of 6⁶.     

Synthesis and structure of dimethyl 3-(2-furoyl)pyrazole-4,5-dicarboxylate

1,3-Dipolar cycloaddition to the diazomethine grouping takes place in the reaction of 2-diazoacetylfuran with dimethyl acetylenedicarboxylate. The structure of the crystalline reaction product, viz., dimethyl 3-(2-furoyl)pyrazole-4,5-dicarboxylate, was investigated by x-ray diffraction analysis. The entire molecule, except for one of the two CO₂CH₃ groups, forms a planar conjugated system. The spectral characteristics of the synthesized compounds are presented.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 1, pp. 91–94, January, 1982.     

Molecular sheets in the crystal structure of a Ba(II) complex with imidazole-4,5-dicarboxylate and water ligands

The structure of poly-tetraaquabis(μ-Himidazole-4,5-dicarboxylato-N,O;-O′)barium(II) dihydrate, Ba(C₅H₃N₂O₄)₂(H₂O)₄·2H₂O is built of molecular sheets in which singly-deprotonated imidazole-4,5-dicarboxylate [H(4,5-IDA)] bridges metal ions using its N, O bonding moiety and one oxygen atom of its second carboxylate group. Each barium(II) is coordinated by N, O bonding moieties of two ligands, two carboxylate oxygen atoms of two other ligands and four waters. The coordination number of Ba(II) is ten, and the coordination polyhedron contains fourteen faces. A network of hydrogen bonds is responsible for the stability of the crystal.     

Hydrothermal synthesis,crystal structure and magnetic properties of a copper(II) phosphonate

The treatment of 3-ammonium-1-hydroxypropylidene-1,1′-bisphosphonate (H₇ahdp) and 4,4′-bipy with CuCl₂?·?2H₂O resulted in a metal phosphonate [Cu(H₅ahdp)?·?H₂O] _n . Its crystal structure has been characterized by single X-ray crystallography. Although there is no 4,4′-bipy in the lattice structure, it plays a very important role in forming the one-dimensional chain of the polymer. Hydrogen bonds link the chains into a 3D network. The dinuclear secondary building units are observed in the compound. The determination of variable-temperature magnetic susceptibilities (5?～?300?K) shows weak intrachain antiferromagnetic coupling between copper(II) centers. The magnetic data were fitted to the appropriate equations derived from the Hamiltonian H?=??2JS ₁ S ₂, giving the parameter J?=??25.78?cm^?1. Its thermal properties were also investigated.     

Hydrothermal synthesis and crystal structures of Mn(II) and Cd(II) aminophosphonates with a layered structure

Two new divalent metal aminodiphosphonates with a layered structure, Mn₂[(HL)(H₂O)F]·H₂O (1) and Cd_3.5[(HL)L] (2) (H₄L =?CH₃CH₂CH₂N(CH₂PO₃H₂)₂), have been hydrothermally synthesized and characterized by single-crystal X-ray diffraction as well as with infrared spectroscopy, elemental analysis and thermogravimetric analysis. In 1, two MnO₄F₂ and two MnO₅F polyhedra are interconnected via edge-sharing into a tetramer, and such tetramers are bridged by the diphosphonate ligands into a Mn(II) phosphonate layer in the ab-plane. The structure of 2 also features a 2D layered structure, in which the CdO₅N and CdO₆ polyhedra are interconnected into a 1D chain. The chains are then cross-linked via phosphonate oxygen atoms to form Cd(II) phosphonate layers in the ab-plane.     

Hydrothermal synthesis,crystal structure and characterization of a 1D neodymium(III) coordination polymer containing the pyridine-2,6-dicarboxylate and oxalate ligands

The reaction of 2,6-pyridinedicarboxylic acid (H₂Pydc) and ammonium oxalate with neodymium(III) nitrate affords the one-dimensional (1D) neodymium coordination polymer formulated as {[Nd₂(Pydc)₂(μ₂-C₂O₄) · 6H₂O] · 2H₂O} _n (I), and characterized by elemental analysis, IR spectroscopy, and X-ray single-crystal diffraction. The complex presents 1D stair-like chain array bridged through oxalate, and these 1D chains are further linked into 3D supramolecular architecture by extensive intra- and intermolecular hydrogen-bonding interactions. Preliminary magnetic studies reveal the presence of weak antiferromagnetic couplings with the two adjacent magnetic centers bridged through the pyridine dicarboxylate oxygen atom in the complex.     

三维超分子化合物(H2bimb)2(SiW12O40)的水热合成与晶体结构

利用水热合成方法合成了1个新的Keggin基质的超分子化合物(H2bimb)2(SiW12O40),并通过元素分析、红外光谱、热重分析和X射线单晶衍射方法确定了该化合物的晶体结构.结构分析表明该化合物属于三斜晶系,P-1空间群,晶胞参数a=1.122 6(5)nm,b=1.563 5(5)nm,c=1.892 7(5)...     

一个新的三维超分子配位聚合物[Ni(pyridine-2-carboxylate)_2]_n·2nH_2O的水热合成及晶体结构

采用水热法合成了一个新的金属-有机配位聚合物[Ni(pyridine-2-carboxylate)2]n·2nH2O,对其进行元素分析、红外光谱和X射线单晶衍射测定.结构分析表明:该晶体属于三斜晶系,P-1空间群,晶胞参数a=5.128 4(6) nm,b=7.634 6(9) nm,c=9.229 5(11) nm,α=74.902(2)°,β=84.347(2)°,γ=71.442(2)°,V=330.70(7) nm3,化学式为C12H12NiN2O6,Mr=338.95,Dc=1.702 g/cm3,μ(Mo,Kα)=1.497 mm-1,F(000)=174,Z=1,R=0.033 3,wR=0.038 4((I＞2σ(I)).并且该配合物通过O-H...O和C-H...O氢键形成了三维超分子网状结构.     

Hydrothermal synthesis and crystal structure of a novel 2-D polymeric manganese (II) complex with mixed ligands

A novel polymeric complex, [Mn(phen)(pdc)]_∞ (phen=1,10-phenanthroline, H₂pdc=2,5-pyridinedicarboxylic acid) has been synthesized from the hydrothermal reaction system of H₂pdc, phen, MnO₂, and H₂O. [Mn(phen)(pdc)]_∞ is characteristic of an edge-sharing dinuclear Mn^II structure unit bridged by pdc, leading to a 2-D framework whose stacking is based on weak H-bond interaction. The temperature dependence of the magnetic susceptibility for [Mn(phen)(pdc)]_∞ indicates antiferromagnetic coupling [J = −2.76(4) cm⁻¹] between the adjacent paramagnetic Mn^II ions.     

A new 3D nickel(II) framework composed of large rings: Ionothermal synthesis and crystal structure

Ionothermal reaction between Ni²⁺ and 1,3,5-benzentricarboxylic acid (H₃BTC) with [AMI]Cl (AMI=1-amyl-3-methylimidazolium) as the reaction medium produced a novel 3D mixed-ligand metal-organic framework [AMI][Ni₃(BTC)₂(OAc)(MI)₃] (1) (MI=1-methylimidazole) with [AMI]⁺ incorporated in the framework. The framework is formed by connecting 2D planes, made up of 32- and 48-membered rings, through 1D chains composed of 32-membered rings. The two BTC³⁻ ligands in 1 show the same connectivity mode with two bidentate and one μ₂ bridging carboxylic groups. This is a new connectivity mode to the already existing 17 in the Ni-BTC system. The role of MI and [AMI]Cl in the structure formation is discussed.     

Hydrothermal synthesis, crystal structure, and photoluminescence of a new 2D cadmium(II) complex: {Cd(C8H5O3Cl2)2(C10H8N2)} n

One new cadmium coordination polymer, [Cd(2,4-Dcp)₂(4,4-Bipy)] _n (I) (2,4-HDcp = 2,4-dichlorophenoxyacetic acid, 4,4′-Bipy = 4,4′-bipyridine) with 2D layer structure, has been prepared by the hydrothermal synthesis and characterized by elemental analysis, IR, TGA and single-crystal X-ray diffraction. Complex I crystallizes belong to monoclinic system and has C2/c space group. Each Cd²⁺ ion is six-coordinated and located at an octahedral geometry. The Cd²⁺ ions are linked by bidentate 2,4-Dcp groups into a linear chain in which the benzene rings of 2,4-Dcp ligands point alternately up and down. These chains are further connected into a sandwich-like layer though 4,4′-Bipy ligands. Furthermore, the photoluminescence and life-time of I in the solid state have been studied.     

Hydrothermal synthesis and crystal structure of a new two-dimensional zinc citrate complex

A new two-dimensional compound C₁₂H₁₄O₁₆Zn₃ (1), containing seven-coordinate zinc atoms was prepared by the hydrothermal technique. The compound obtained was characterized by TG-DTA, single crystal X-ray diffraction, elemental analysis and FT-IR analysis. Single-crystal X-ray diffraction analysis shows that compound 1 crystallizes with monoclinic symmetry in the space group P2₁/c, a?=?6.1552(13)?Å, b?=?14.546(3)?Å, c?=?9.581?Å, β?=?102.66(2)°, V?=?836.9(4)?ų, Z?=?2, R1?=?0.0311, wR2?=?0.0830.     

[Co(1,10-phen)(H_2O)(VO_3)_2]的水热合成、结构及电化学性质

采用水热方法并以邻菲啉为模板剂合成了一种过渡金属配合物连接的无机-有机层状结构的多金属钒酸盐Co(1,10-phen)(H2O)(VO3)2,该化合物经过X-射线单晶衍射、元素分析、红外光谱表征和热失重分析,并用循环伏安法研究了标题化合物的电化学性质.     

Hydrothermal synthesis,crystal structure and antibacterial studies of nickel(II) and manganese(II) complexes with ciprofloxacin

Hydrothermal treatments of ciprofloxacin with Ni(NO₃)₂·6H₂O and Mn(ClO₄)₂·6H₂O yield two metal complexes: [Ni(H-cip)₂(H₂O)₂](NO₃)₂·2H₂O (1) and [Mn(H-cip)₂(H₂O)₂] (ClO₄)₂·2H₂O (2), confirmed by elemental analysis, IR and single crystal X-ray diffraction analyses. Complexes 1 and 2 were screened for antibacterial activity against Staphylococcus aureas, E. coli, Pseudomonas aeruginos and Candidaalbicans.