Synthesis of a new aza-14-crown-4 with di(α-pyridyl)-substituted bispidine subunit and the crystal structure of its complex with CoCl2

The aza-14-crown-4 with the di(α-pyridyl)-substituted bispidine subunit (L) and its cationanion complex with cobalt(II) chloride of composition [Co(L)(H₂O)][CoCl₄] (I) have been synthesized. The structure of compound L has been proved by IR spectroscopy, NMR, and mass spectrometry. X-ray crystallography has demonstrated that the L molecule in the complex is an NNNN-tetradentate chelating ligand, and the crown ether moiety is not directly bound to the metal cation. In the cationic moiety of the complex, the Co(1) atom has an octahedral environment, and the Co(2) polyhedron in the anionic moiety is a tetrahedron. The cationic and anionic moieties of complex I are linked by the bridging chlorine atom.     

Synthesis and crystal structure of dinuclear nickel (Ⅱ) complex

The crystal structure of Ni(Ⅱ) complex with 3-hydroxyl-1, 5-diazacycloheptane-N, N'-diacetate was determined by X-ray diffraction method. Crystal data for Ni2 (C9H14N2O5)2·2H2O: monoclinic, space group P21/n, a = 1.1717(5), b = 0.9794(3), c = 1.2971(2) nm, β= 96.62(3), V= 1.4786(7) nm3, Dc = 1.377 g/cm3, Z = 2,μ=13.321 cm-1 (Mo-Kα), F(000)=640. The final R and Rw are 0.075 and 0.089 respectively. The Ni(Ⅱ) ion forms 2:2 complex with ligand. Two ligands are bridged by two Ni(Ⅱ) atoms which are bridged by two O atoms. Every Ni(Ⅱ) is coordinated by two N atoms and four 0 atoms. The coordination polyhedron of the Ni(Ⅱ) ion is a distorted octahedron.     

Cobalt(II) hexaiododimercurate(II) complex with ε-caprolactam: Synthesis and crystal structure

The conditions of synthesis of a new binary complex salt [Co(Cpl)₆][Hg₂I₆] (Cpl is ε-caprolactam ε-C₆H₁₁NO) have been developed, and its structure has been characterized. The salt crystallizes in triclinic system, space group \(P\bar 1\), a = 10.1078(4) Å, b = 12.2680(5) Å, c = 13.0782(5) Å, α = 62.872(2)°, β = 72.394(2)°, γ = 76.834(2)°, V = 1367.98(9) ų, Z = 1, and ρ_calc = 2.297 g/cm³. The structure is insular and consists of isolated ions.     

Synthesis and crystal structure of π complex of copper(I) chloride with diallyl trisulfide 2CuCl · DATrS

Crystals of the π complex 2CuCl·DATrS (DATrS = diallyl trisulfide) were prepared by ac electrochemical synthesis and studied by X-ray diffraction. The crystals are monoclinic, space group C2, Z = 2, a = 12.737(1) Å, b = 5.0984(5) Å, c = 8.9263(7) Å, β = 101.159(5)°, V = 568.72(8) ų. The structure contains infinite coils of (CuCl)_n, which are united into a three-dimensional structure by the bibridge tetradentate ligand DATrS symmetric to axis 2. The trigonal-pyramidal surrounding of the Cu atom consists of two Cl atom, the olefine C=C group, and the S atom (in the apical position) of different DATrS molecules.     

Synthesis of a new complex Chromium (Ⅲ) 2-mercaptonicotinate

Chromium is an essential trace element for mammals[1-3].Diabetes is a chronic disease with major health consequence.Studies show that the occurrence of diabetes have great thing to do with the chromium deficient。Almost 40 years after the first report of glucose tolerance factor(GTF) [4] no conclusive evidence for an isolable ,biologically active form of chromium exited。Three materials have been proposed to be the biologically active form of chromium:“glucose tolerance factor”,chromium Pi…     

Synthesis,crystal structure,and magnetic properties of a salt containing [Cu2Cl7]3− and 4-nitrobenzyl-4′-dimethylaminopyridinium

A new salt, [NO₂BzDMAP]₃[Cu₂Cl₇]?·?H₂O (1), has been synthesized, where [NO₂BzDMAP]⁺ is 1-(4′-nitrobenzyl)-4-dimethylaminopyridinium. Herein, the synthesis, spectral and structural characterization, and magnetic behavior of 1 are reported. It is orthorhombic, with space group Pca2₁, and a?=?26.639(2)?Å, b?=?9.638(1)?Å, and c?=?20.011(2)?Å with V?=?5137.5(7)?ų for Z?=?4. The anion shows a chloride-bridged binuclear structure with Cu?···?Cu distance of 3.872?Å; the two Cu(II) ions have a tetrahedral geometry. The cations stack through p?···?π and π?···?π interactions, and a complicated hydrogen-bonding network structure is formed through C–H?···?Cl and C–H?···?O hydrogen bonds. The variable temperature magnetic susceptibility measurements reveal that 1 exhibits strong antiferromagnetic interaction with J?=??193.0?cm^?1.     

Synthesis and crystal structure of a heterodinuclear complex with a bridged ethenyl ligand FeCo(CO)7(μ-CH=CPhH)

[Fe₂(CO)₆(μ-CO)(μ-CHCPhH)]⁻ reacts with Co₂(CO)₈ at room temperature to give the neutral heterodinuclear complex FeCo(CO)₇(μ-CHCPhH), which has been characterized by elemental analysis and spectroscopic (mass, IR and ¹H NMR) methods and by determination of its structure by X-ray diffraction.     

Synthesis,properties, and crystal structures of a new charge-transfer salt: Tris (dimethylammonium) hydrogen α-dodecamolybdosilicate

A new charge-transfer salt, [(CH₃)₂NH₂]₃[HSiMo₁₂O₄₀] (I), has been synthesized and characterized by elemental analysis, IR, UV-Vis, XPS, TG-DTA, and single-crystal X-ray diffraction. Crystal data: trigonal, R \(\bar 3\) m, a = 16.4365(8), c = 25.142(2) Å, V = 5882.3(7) ų, Z = 6. The X-ray crystallographic study shows that the title compound comprises three (CH₃)₂NH ₂ ⁺ cations and a heteropolyanion and is formed mainly by electrostatic interactions, hydrogen bonding being very weak. The title compound shows weak photochromic properties on UV irradiation. The TG-DTA curves suggest that I is stable up to 300°C     

Synthesis and crystal structure of a neutral open framework cobalt(II) phosphate Co6(PO4)4·7H2O with a channel structure

Using tri-ethyl phosphate as a phosphate source, the hydrothermal reaction of cobalt(II) oxalate di-hydrate, zinc oxide and 1,8 di-amino octane at 200°C gave purple crystals of Co₆(PO₄)₄?·?7H₂O (1), along with a mixture of open-framework zinc–cobalt phosphates Co–Zn–HPO₄, and Co₃(HPO₄)₂(2OH). Compound 1, has been characterized by thermal analysis, FTIR and single crystal X-ray diffraction. The single crystal structure of Co₆(PO₄)₄?·?7H₂O reveals cobalt in four, five and six-fold coordination with linkages through the bridging water molecules and the oxygen atoms of the phosphate in the subunits. Four subunits are connected together through the oxygen atoms (PO₄), to form the three dimensional open framework structure, with a 20-member ring channel that hosts two uncoordinated water molecules. Thermal removal of the water molecules occurs between 400–600°C, with the collapse of the structure above 600°C.     

Synthesis and crystal structure of cobalt(III) α-dioximates with pyrazine

A series of new coordination compounds of cobalt(III) trans-dioximates with pyrazine [CoCl(DH)₂Pz] · H₂O (I), [CoBr(DH)₂Pz] · H₂O (II), [Co(DH)₂Pz₂]NO₃ · H₂O (III), [Co(DH)₂Pz₂][BF₄] (IV), [Co(MgH)₂Pz₂][BF₄] (V), and [Co(NioxH)₂Pz₂][BF₄] (VI), where DH, MgH, and NioxH are dimethylglyoxime, methylglyoxime, and 1,2-cyclohexanedionedioxime monoanions, respectively, Pz is a pyrazine molecule were synthesized. The structures of compounds I, II, and VI were determined by X-ray diffraction. The Co(III) environment in these compounds is octahedral and the pseudomacrocyclic (DioxH⁻)₂ fragment occurs in the equatorial plane. This fragment is stabilized by O-H…O hydrogen bonds. The neutral Pz ligand is monodentate in all three compounds.     

Synthesis,X-ray crystal structure,electrochemical and antibacterial activity of a silver(I) complex with α-bromo-cinnamaldehyde salicylhydrazone

The mononuclear silver(I) complex [AgL(HL)·DMF] (I) (HL = C₆H₁₃O₂N₂Br) has been prepared and characterized by physicochemical and spectroscopic methods, single crystal X-ray diffraction, cyclic voltammetry, and antibacterial activity tests. The complex crystallized in the triclinic system, and each Ag(I) is six-coordinate with a distorted octahedral geometry. The ligands chelate the metal center with N, O, and Br atoms from two different Schiff base ligands. O–H···O intermolecular hydrogen bonds connect adjacent complex molecules to form zigzag one-dimensional linear chains along the b axis. Cyclic voltammetry showed that the complex displays an irreversible reduction process at −0.41 V. The data from antibacterial activity tests indicate that the complex inhibits the growth of Staphyloccus aureus and Bacillus subtilis Cohn.     

Synthesis,crystal structure,antibacterial activities,and DNA-binding studies of a new μ-oxamido-bridged binuclear copper(II) complex

A new μ-oxamido-bridged dicopper(II) complex, Cu₂(heap)(NO₃)₂ (1), where heap is the dianion of N,N′-bis(N-hydroxyethylaminopropyl)oxamide, has been synthesized and characterized by elemental analysis, molar conductivity, IR and electronic spectral studies, and X-ray single-crystal diffraction. The complex consists of a neutral centro-symmetric binuclear copper(II) unit with an inversion center at the midpoint of the Cl?Clⁱ bond. The copper(II) has square-pyramidal coordination geometry and the bridging heap adopts a bis-tetradentate conformation. The binuclear units are linked into a 3-D framework by N?H ··· O, O?H ··· O, and C?H ··· O hydrogen bonds. Due to weak coordination between copper(II) and nitrate, the neutral dicopper(II) units are present as binuclear cations and nitrate anions in solution. Antibacterial assays indicate that the complex shows better activity than the ligand. Interactions of the complex with herring sperm DNA (HS-DNA) have been investigated by using cyclic voltammetry, UV absorption titrations, ethidium bromide fluorescence displacement experiments, and viscometry measurements. The results suggest that the binuclear copper(II) complex interacts with HS-DNA by electrostatic interaction with intrinsic binding constant of 3.33 × 10⁴ M^?1.     

Synthesis and crystal structure of Co(III) dioximates with the complex anion [SbF6]?

The complexes [Co(DioxH)₂L₂][SbF₆] · nH₂O, where DioxH is dimethylglyoxime monoanion (DioxH^?) or 1,2-cyclohexanedione dioxime (NioxH^?), L is aniline (An) or triphenylphosphine (PPh₃), were isolated from the CoX₂ · nH₂O-NaSbF₆-DioxH₂-L system (X = F or CH₃COO) in aqueous methanol. The complexes were studied by UV, IR, and NMR spectroscopy and by X-ray diffraction. The crystal structure of [Co(DH)₂(An)₂][SbF₆] · H₂O (I) and [Co(NioxH)₂(PPh₃)₂][SbF₆] (II) is stabilized by the electrostatic interactions between the Co(III) complex cations and outer-sphere fluorine-containing anions and by hydrogen bonds between structural units.     

Synthesis and crystal structure of a new polpouclear complex with a monomer of (3,4,9,10-dibenzo-1, 12-diaza-5, 8-dioxacyclopentadecane)-copper(Ⅱ) (μ-Cl)_2 zinc(Ⅱ) chloride

A polynuclear complex containing a monomer of Cu(Ⅱ)-Zn(Ⅱ) heterobinuclear unitwas synthesized and characterized by IR spectra and magnetic moment. The crystal and molecularstructure of the complex, CuZnC_(19)H_(24)Cl_4N_2O_2, was determined by X-ray diffraction, it crystallizedin monoclinic, P2_1 / m, a = 8.812 (2), b = 15.972(3), c = 8.831(1) A, β = 114.33(1)°, V = 1132.4A~3,Z=2, D_c= 1.710 g / cm~3, λ(Mo K_α) = 0.71073A, μ = 25.227 cm~(-1), R = 0.051. R_w = 0.063 for 1130 ob-served reflections with I> 3σ(I) . The coordinated octahedra of Cu(Ⅱ) and tetrahedra of Zn(Ⅱ) viabridging Cl atoms form a single chain polynuclear complex. The Cu, Zn and bridging Cl atoms arelocated on the crystallographic symmetry plane m which is perpendicular to 2N and 2O donor plane.     

Synthesis,crystal structure and magnetic properties of [1-(4′-bromobenzyl)-4-methylquinolinium] [Ni(mnt)2] complex (mnt2 − =maleonitriledithiolate)

A new ion-pair complex, [BrBzMeQl][Ni(mnt)₂] (1) ([BrBzMeQl]⁺?=?1-(4′-bromobenzyl)-2-methylquinolinium; mnt^2??=?maleonitriledithiolate), has been prepared and characterized. X-ray diffraction analysis shows that the Ni(mnt)₂ anion and [BrBzMeQl]⁺ cations of 1 form completely segregated stacking columns, with the Ni?···?Ni distances alternating between 3.717 and 4.466?Å?in the Ni(mnt)₂ stacking column. The variable-temperature magnetic susceptibilities of 1 have been measured over the range 75–300?K and the results reveal that the complex exhibits antiferromagnetic behavior.     

Synthesis and structure of a ‘4 + 1’ oxorhenium(V) complex containing imidazole derivatives

The ‘4?+?1’ concept was used to prepare the complex salt [ReO(iao)Br]Br (1) from the reaction of (n-Bu₄N)[ReOBr₄(OPPh₃)] with the ligand bis{2′-methyl(1′-methylimidazole)}-2-aminoethanol (Hiao) in methanol. The single-crystal X-ray crystal structure of 1 shows that iao acts as a monoanionic, tetradentate, N₃O-donor chelate. When the reaction was carried out in acetonitrile, the neutral complex [ReO(iao)Br₂] (2) was isolated. Elemental analyses and IR data suggest that iao acts as a tridentate, N₂O-donor ligand in 2.     

Synthesis,crystal structure,and properties of a new cadmium(ΙΙ) polymer with mixed Cl−/SCN− ligands: [CdCl(SCN)] n

A 1-D chain complex, cadmium(ΙΙ) chloride thiocyanate (1), [CdCl(SCN)] _n was synthesized by evaporation and characterized by single-crystal X-ray diffraction and FT-IR techniques. The compound crystallizes in the space group Pnma of orthorhombic system with cell parameter a = 9.5967(7), b = 4.2595(3), and c = 10.1789(7) Å; V = 416.08(5) ų and Z = 4. The cadmium(ΙΙ) is five-coordinate, surrounded by one pair of (µ-1,1-NCS) bridging NCS^? and three Cl^? as a µ₃-linker coordinating three Cd(ΙΙ) centers, approximately a severely distorted square-pyramidal configuration. Cd(ΙΙ), Cl^?, and SCN^? form an infinite 1-D chain with chair-like features, a new example of mixed Cd–NCS–Cl discrete compounds. The photophysical properties of the crystals have been investigated with one emission peak at 473 nm observed for the title complex in the solid state, which exhibits blue luminescence. The mechanical properties of the crystals have been studied using Vickers microhardness tester and the hardness was 78.6 kg mm^?2.