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1.
A novel three-dimensional cobalt(II)-radical complex {Co(NITmPy)2[N(CN)2]2}n (NITmPy = 2-(3′-pyridyl)-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide) is prepared and characterized by X-ray crystallography. The complex crystallizes in the monoclinic system, space group P21/c, with unit cell parameters a = 12.5775(5) Å, b = 10.9340(5) Å, c = 11.6134(5) Å, β = 108.1320(10)°; V = 1517.79(11) Å3, ρcalcd = 1.443 g/cm3, and Z = 2 for R 1 = 0.0463. In the complex, each cobalt ion is six-coordinate with four nitrogen atoms from four N(CN) 2 t- ligands and two nitrogen atoms of pyridyl groups, and the [Co(NITmPy)2]2+ units are linked by N(CN) 2 t- μ-bridging ligands to form a three-dimensional structure. The variable-temperature magnetic susceptibility data show that the complex exhibits weak antiferromagnetic interactions.  相似文献   

2.
A novel bridging ligand, (3,5-dichloropyridin-4-yl)(pyridin-4-yl)methanol (I), and its cobalt(II) complex, [Co(I)2(NCS)2]n (II), were prepared. The structures of ligand I and complex II were determined by single crystal X-ray analysis. Magnetic susceptibility measurements were performed for cobalt (II) complex II. Compound I crystallised in orthorhombic space group Pbca with a = 7.6585(14) Å, b = 12.209(2) Å, c = 23.207(4) Å, V= 2170.0(7) Å3 and Z=8. Complex II crystallised in monoclinic space group P21/n with a = 13.223(8) Å, b = 16.959(10) Å, c = 13.948(8) Å, β = 115.395(10)°, V= 2826(3) Å3 and Z = 4. Each cobalt(II) ion is surrounded by two NCS? anions and four pyridyl moieties from two bridging ligands. Each bridging ligand connects two neighbouring Co(II) ions to form a 2-dimensional structure. Temperature dependence of the molar magnetic susceptibilities in the temperature range of 2–300 K revealed that magnetic interactions between the cobalt ions are weak.  相似文献   

3.
A new manganese(II) complex [MnCl2(NIT-1′-MeBzIm)2] · 3H2O (NIT-1′-MeBzIm = 2-{2′-[(l′-methyl)benzimidazolyl]}-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide) has been prepared and structurally characterized by single-crystal X-ray diffraction. The complex crystallizes in monoclinic, space group C2/c, Z = 4. Crystal data: C30H38Cl2MnN8O8, M = 764.52, a = 17.261(3) Å, b = 21.317(4) Å, c = 11.744(2) Å, β = 108.464(2)°. The X-ray analysis reveals that Mn(II) atom is six-coordinated with a distorted octahedral geometry. The complex was linked by intermolecular hydrogen bonds, leading to a 2D network configuration. Magnetic investigation indicates the existence of interamolecular interactions is ferromagnetic with J = 1.11 cm?1.  相似文献   

4.
The coordination compound [Co(L)(Mal)(H2O)2]H2O (I) (L is benzhydrazide, H2Mal is malonic acid) has been synthesized and studied by IR spectroscopy, thermogravimetry, and X-ray diffraction. Crystals are triclinic, a = 7.610(4) Å, b = 7.854(2) Å, c = 12.751(2) Å, α = 75.12(3)°, β = 88.01(3)°, γ = 80.26(3)°, Z = 2, space group \(P\bar 1\). The structure is molecular. The Co2+ atom has a distorted octahedral coordination. The Co-O and Co-N bond lengths are 2.031-2.129(4) and 2.157(5) Å, respectively. The endocyclic O1Co1N1 bond angles are 77.3(2)° and 90.0(2)° in the five- and six-membered chelate rings, respectively. Molecules of complex I are linked via a great number of hydrogen bonds. The C…C contacts between phenyl rings additionally strengthen the structure.  相似文献   

5.
The binuclear manganese(II) complex of formula [Mn2(CHZ)2(H2O)2(SO4)2] (CHZ = carbohydrazide) (1) has synthesized in aqueous solution and characterized by elemental analysis, IR, and single crystal X-ray diffraction. The compound 1 crystallizes in monoclinic system, space group P2(1)/n, a = 7.083(1) Å, b = 7.985(1) Å, c = 14.045(2) Å, β = 90.46(1)°, V = 794.42(16) Å3, Z = 2, R = 0.0308 with 1481 reflections. In the title complex, two Mn(II) cations are bonded via the bridging oxygen atoms into a centrosymmetric dimeric unit. The Mn(II) dimers are further extended into layers by means of the bridging sulfate groups. Each Mn atom in the complex is in bivalent state with a distorted pentagonal bipyramid configuration and has a N2O5 donor set which consists of two nitrogen atoms and five oxygen atoms provided by the ligands of two CHZ molecules, one water molecule, and two sulfate ions. The CHZ tridentate ligands are coordinated with adjacent Mn(II) cation via two terminal N atoms and the carbonyl O atom and sulfate anions act as bidentate bridge ligand. Four kinds of Mn(II) CHZ complex structures are compared. The thermal property of title complex was studied by using DSC and TG-DTG techniques. The results exhibit the title complex is highly stable.  相似文献   

6.
The crystal structure of 1,10-phenanthroline-5,6-dione ligand with Zn(II), tris(1,10-phenanthroline-5,6-dione)zinc(II) hexafluorophosphate, [Zn(phen-dione)3](PF6)2, is reported. The complex was characterized by elemental analysis, IR, 1H NMR, electronic absorption spectroscopies, cyclic voltammetry and X-ray crystallography. Yellow crystals of [Zn(phen-dione)3](PF6)2 were formed by ether diffusion into an acetonitrile solution of the complex. The title complex crystallized in monoclinic crystal system (Z = 2) with space groups of P2 1, a = 12.0299(15) Å, b = 14.5306(19) Å, c = 13.1879(17) Å, β = 94.058(2)º and V = 2299.5(5) Å3. The structure was refined by using 10048 independent reflections, with I > 2σ(I) to an R factor of 0.0490. Single-crystal structure showed that the coordination geometry around the Zn(II) was a distorted octahedron. The complex showed an intense fluorescence band at visible region (690 nm) in CH3CN with an excitation wavelength of 310 nm at 25.0 ± 0.1 ºC. Cyclic voltammogram of the title complex showed two quasi-reversible reduction couples at negative potential, which were assigned to the consecutive reduction of phen-dione ligand to phen-semiquinonate and phen-diolate respectively by analogy to other phen-dione complexes at scan rate 200 mV s-1.  相似文献   

7.
Interaction of Co(II) chloride with optically active bis-pinane propylenediaminodioxime (H2L) gave a diamagnetic compound of Co(III) with a composition [Co(HL)Cl2]. The crystal and molecular structure of the compound was determined by X-ray diffraction (XRD) analysis (Enraf-Nonius CAD-4 diffractometer, λMoKα, 703 F hkl , R = 0.0347). The crystals are orthorhombic with unit cell parameters a = 8.989(1) Å, b = 12.351(2) Å, c = 22.425(3) Å, V = 2487.7(6) Å3, Z = 4, ρcalc = 1.420 g/cm3, space group P212121. The crystal structure of the complex is composed of discrete one-center molecules. In the complex, the Co3+ ion coordinates four N atoms of the tetradentate cycle-forming ligand (HL? anion) and two Cl atoms. The coordination polyhedron of Co is a distorted octahedron Cl2N4.  相似文献   

8.
The self-assembly of unsymmetrical tecton 3-nitro-5-(pyridin-4-yl)benzoic acid (HL)with cobalt chloride under hydrothermal conditions affords a new 2D coordination polymer [Co(L)2] n (1, L = 3-nitro-5-(pyridin-4-yl)benzoate), which is characterized by elemental analysis, infrared spectroscopy, thermogravimetric analysis, powder X-ray diffraction analysis, and single crystal X-ray diffraction. Compound 1 is of the triclinic system, space group P-1 with a = 9.7857(12) Å, b = 10.3417(13) Å, c = 10.8463(13) Å, α = 85.155(2)°, β = 74.785(2)°, γ = 88.962(2)°, V = 1055.4(2) Å3. The crystal structural analysis of complex 1 shows that the cobalt center is six-coordinated in an octahedral geometry by four O atoms from four different L ligands and two N atoms from two different L ligands; the Co(II) cations are bridged by μ3-L into an interesting two-dimensional network structure. It should be pointed out that the thermal analysis results indicate that complex 1 is quite stable up to 420°C.  相似文献   

9.
The structure, spectroscopic, and electrochemical properties of [Co{(Me-sal)2dien}(N3)] and [Co{(Me-sal)2dpt}(N3)], where (Me-sal)2dien = 2,2′-[1,1′-(3-azapentane-1,5-diyldinitrilo)diethylidyne] diphenolate and (Me-sal)2dpt = 2,2′-[1,1′-(4-azapentane-1,7-diyldinitrilo)diethylidyne] diphenolate, have been investigated. These complexes have been characterized by elemental analyses, IR, UV–Vis, and 1H-NMR spectroscopy. The crystal structures of these complexes have been determined by X-ray diffraction. Complex 1 crystallizes in the triclinic space group P 1, with a = 7.8443(4) Å, b = 11.0660(5) Å, c = 11.6216(6) Å, α = 73.360(1)°, β = 76.965(1)°, γ = 84.436(1)° and Z = 2. Complex 2 crystallizes in the monoclinic space group P21/n, with a = 12.1985(13) Å, b = 10.9332(12) Å, c = 15.2808(16) Å, β = 76.965(1)° and Z = 4. The coordination geometry around cobalt(III) in both complexes is a distorted octahedron. The electrochemical reduction of these complexes at a glassy carbon electrode in acetonitrile indicates that the first reduction corresponding to CoIII–CoII is electrochemically irreversible, accompanied by dissociation of the axial Co–N(N3) bond. The second reduction step of Co(II/I) leads to decomposition of the complex. These observations are rationalized based on the structure-function relations.  相似文献   

10.
The coordination compounds [CoL2Cl2] (I) and [CdL2(H2O)2(NO3)2] (II) have been synthesized by the reaction of CoCl2 · 6H2O and Cd(NO3)2 · 4H2O with L = 2-amino-4-methylpyrimidine (Ampym, C5H7N3), and their structures have been solved. The crystals of complex I are triclinic, space group $P\bar 1$ , a = 5.627(1) Å, b = 11.191(1) Å, c = 12.445(1) Å, α = 81.00(1)°, β = 77.21(1)°, γ = 76.18(1)°, V = 737.7(2) Å3, ρcalcd = 1.567 g/cm3, Z = 2. The crystals of complex II are monoclinic, space group P21/c, a = 10.390(1) Å, b = 11.982(1) Å, c = 7.624(1) Å, β = 102.61(1)°, V = 926.1(2) Å3, ρcalcd = 1.760 g/cm3, Z = 2. Discrete [CoL2Cl2] moieties are realized in the structure of complex I. The cobalt atom is tetrahedrally coordinated to the two nitrogen atoms of crystallographically nonequivalent ligands L and two chlorine atoms (Co(1)-Navg, 2.051(4)Å; Co(1)-Cl(1), 2.241(1) Å; Co(1)-Cl(2), 2.263 Å; bond angles at the cobalt atom lie within a range of 102.1°–118.6°). The complexes are linked into supramolecular zigzag chains by N-H...N(Cl) hydrogen bonds. In the structure of complex II, the Cd2+ ion (at the inversion center) is coordinated in pairs to the nitrogen atoms of ligand L and the O(NO3) and O(H2O) oxygen atoms. The coordination of the Cd2+ ion is distorted octahedral (Cd(1)-N(1), 2.341Å; Cd(1)-O(1), 2.340(4) Å; Cd(1)-O(4), 2.327(3) Å; bond angles at the cadmium atom lie within a range of 79.1°–100.9°). N-H...N hydrogen bonds link the complexes into supramolecular chains. These chains are linked into a supramolecular framework by the O-H...O hydrogen bonds between water molecules and NO3 groups.  相似文献   

11.
A new Schiff base cobalt(III) complex with the formula [CoL1L2(N3)]·NO3 (L1 is 2-[1-(2-phenylaminoethylimino)ethyl]phenolate, L2 is N-phenylethane-1,2-diamine) is prepared and characterized by physicochemical methods and single crystal X-ray determination. The complex crystallizes in the triclinic system space group P-1, with a = 8.504(2) Å, b = 14.973(3) Å, c = 20.676(4) Å, α = 100.021(3)°, β = 90.005(3)°, γ = 103.084(2)°, V = 2523.0(9) Å3, Z = 4, R 1 = 0.0732, and wR 2 = 0.1182. Single crystal X-ray diffraction analysis reveals that the complex contains two mononuclear [CoL1L2(N3)]+ cations and two nitrate anions. The Co atom is six-coordinated in an octahedral geometry. The ligands and the cobalt(III) complex are screened in vitro for their antibacterial activity against Bacillus subtillis, Staphylococcus aureus, Escherichia coli, and Pseudomonas aereuguinosa.  相似文献   

12.
A single-ligand complex Pd(II)-L-aspartic acid was synthesized and characterized by elemental ana-lysis and IR spectra. The crystal structure of the complex was determined by single crystal X-ray diffraction (crystallizing in orthorhombic crystal system, space group P212121 with unit cell parameters a = 5.3145(11) Å, b = 9.6294(19) Å, c = 22.233(4) Å, and Z = 4). The Pd atom was four-coordinated with N(1), N(2), O(4), and O(5) from two L-aspartic ligands and formed a slightly distorted parallelogram geometry. 2D “zigzag” shaped supramolecular networks are constructed via hydrogen bonding. The binding of the title complex with fish sperm DNA (FS-DNA) has been investigated by absorption and fluorescence spectra and the results indicate that the complex bind to FS-DNA in an intercalative mode. Gel electrophoresis shows the cleavage of both supercoiled and circular pBR322 DNA to form a small molecular fragment under the action of the title complex. The cytotoxicity assay proves that the complex has strong anticancer activity to human cervix epitheloid carcinoma cell lines (HeLa).  相似文献   

13.
A new one-dimensional dicyanamide bridged zinc(II) complex containing nitronyl nitroxide radicals [Zn(Hfac)2(NIT-1′-MeBzIm)] (NIT-1′-MeBzIm = 2-{2′-[(l′-methyl)benzimidazolyl]}-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide, Hfac = hexafluoroacetylacetonate) has been prepared and structurally characterized by single-crystal X-ray diffraction. The complex crystallizes in monoclinic, space group P21/c, Z = 4. Crystal data: C25H21F12N4O6Zn, Mr = 766.83, a = 12.1812(13) Å, b = 16.8770(18) Å, c = 15.5230(16) Å, β = 98.009(2)°, V = 3160.1(6) Å3, ρ c = 1.612 g/cm3, μ(MoK α) = 0.893 mm?1, F(000) = 1540, R = 0.0925 and wR = 0.2652 for 5875 observed reflections with I > 2σ(I). The X-ray analysis reveals that the zinc(II) ion is six-coordinated with a distorted octahedral geometry. These units develop as 1D species by intermolecular hydrogen bonds. Magnetic investigation indicates the existence of weak intermolecular interactions is antiferromagnetic with J = ?1.35 cm?1, where the spin Hamitonian is defined as H = ?2Σ i,j J i,j S i S within the complex.  相似文献   

14.
The crystal structure of the title compound has been solved by X-ray diffraction. [CO(Cl)2(N4C18H36)]-(ClO4), Mr = 537.79, triclinic, P1, a = 6.974(4), b = 8.530(1), c = 11.061(2) Å, α = 98.47(1), β = 106.56(3), γ = 93.02(3)°, V = 620.8(4) Å3, Z = 1, Dx = 1.439 Mg m?3, λ(MoKα) = 0.7093 Å, μ = 0.96 mm?1, F(000) = 291.93, T = 297(3) K, R = 0.072, Rw = 0.085 for 2121 observed reflections. The Co(III) is six-coordinate with the four N atoms of the macrocyclic ligand equatorial and two Cl ions axial, thereby resulting in a tetragonally distorted octahedral geometry. Aside from the perchlorate group, there exists a non-crystallographic inversion center at the Co(III) ion for the macrocyclic ligand and the two Cl ions which are bonded to the Co(III) ion.  相似文献   

15.
A new azido-coordinated nickel(II) complex [NiL1(N3)] (1) and a new thiocyanato-coordinated nickel(II) complex [NiL2(NCS)] (2), where L1 and L2 are the monoanionic forms of Schiff bases 2-[(2-isopropylaminoethylimino)methyl]-6-methylphenol and 2-[(2-dimethlaminoethylimino)methyl]-6-methylphenol respectively, are prepared and structurally characterized by elemental analysis, IR spectra, and single crystal X-ray crystallography. Complex 1 crystallizes in the triclinic space group P-1 with unit cell dimensions a = 8.812(2) Å, b = 9.433(3) Å, c = 9.488(2) Å, α = 81.933(2)°, β = 69.925(2)°, γ = 84.591(2)°, V = 732.5(3) Å3, Z = 2, R 1 = 0.0291, and wR 2 = 0.0734. Complex 2 crystallizes in the monoclinic space group P21/n with unit cell dimensions a = 7.4497(4) Å, b = 6.1933(3) Å, c = 31.5126(18) Å, β = 92.484(2)°, V = 1452.57(13) Å3, Z = 4, R 1 = 0.0307, and wR 2 = 0.0668. The Ni atom in each of the complexes is coordinated by three donor atoms of the Schiff base ligand and by one N atom of the azide or thiocyanate ligand, forming a square planar geometry. The azide and thiocyanate anions readily coordinate to the complexes as secondary ligands.  相似文献   

16.
Complex salts [M(NH3)5Cl](ReO4)2, where M = Cr, Co, Ru, Rh, Ir, have been prepared. The crystal structure of [Rh(NH3)5Cl](ReO4)2 was determined by single crystal X-ray diffraction. Crystal data: a = 17.369(4) Å, b = 7.7990(16) Å, c = 11.218(2) Å, V = 1430.5(5) Å3, space group C2/m, Z = 4, d calc = 3.19 g/cm3, R = 0.0447. Complex salts from the above series are shown to be isostructural; they were defined by X-ray crystallography. Thermal decomposition of the compounds in an inert atmosphere and under hydrogen has been studied. According to X-ray phase analysis (XRPA) data, the M0.33Re0.67 (M = Co, Ru, Rh, Ir) monophase solid solutions are the products of reduction of the salts under hydrogen.  相似文献   

17.
A new binary complex salt — chloropentaamminechromium(III) tetrabromopalladate(II) [Cr(NH3)5Cl][PdBr4] — has been synthesized. The compound was characterized by elemental, X-ray diffraction, and X-ray phase analysis. The salt is isostructural with the previously investigated compounds [M(NH3)5Cl][PtCl4] (M = Ir, Rh, Ru, Co, Cr) and [CM(NH3)5Cl][PdBr4] (M = Ir, Rh, Co). Crystallographic data: space group Pnma, a = 17.068(2) Å, b = 8.315(12) Å, c = 9.653(14) Å; V = 1370.0(3) Å3, Z = 4, d calc = 2.903 g/cm3.  相似文献   

18.
Compounds of the [Co(DH)2A2](BiEdta) · 6H2O type (where DH is the monodeprotonated dimethylglyoxime ON=C(CH3)–(CH3)C=NOH; A is the o-, m-, or p-toluidine; and Edta is the ethylenediaminetetraacetate(4–) ion) were synthesized and studied. The composition and structures of the complexes were determined from their UV and 1H NMR spectra and from X-ray diffraction data. The isomer [Co(DH)2(o-NH2C6H4CH3)2]2[Bi2(μ-Edta)2(H2O)2] · 10H2O was structurally characterized using X-ray diffraction analysis. The crystals are triclinic: a = 12.153(2) Å, b = 12.824(3) Å, c = 16.215(3) Å, α = 67.73(3)°, β = 86.18(3)°, γ = 66.96(3)°, space group P $\overline 1$ , ρ(calcd) = 1.719 g/cm3, Z = 4. The structure is composed of complex binuclear [Bi2(μ-Edta)2(H2O)2]2– anions, [Co(DH)2(o-NH2C6H4CH3)2]+ cations, and molecules of crystallization water. The Edta4– anion chelates with the Bi atom in a hexadentate manner (N2O4); the fifth O atom functions as a bridging ligand. The bismuth coordination polyhedron can be regarded as a strongly distorted antiprism. In the octahedral cation, the Co(III) atom coordinates four N atoms of two DH ligands (average Co–N 1.897 Å) and two N atoms of two o-toluidine molecules (Co–N 2.023 Å). Thermolysis of the complexes studied was found to proceed in several successive steps, namely, the deaquation, deamination, and pyrolysis of the ligands.  相似文献   

19.
Reaction of molybdenyl(IV) oxide bis(2,4-pentanedionate) with N′-(3-ethoxy-2-hydroxybenzylidene)-2-methoxybenzohydrazide in methanol affords a mononuclear dioxomolybdenum(VI) complex containing MoO5N basic core. The complex has been characterized by various physicochemical techniques (IR and elemental analysis), and single crystal X-ray diffraction. X-ray crystal structure determination reveals that the complex crystallizes as monoclinic space group P21/c, with unit cell dimensions a = 9.251(1), b = 11.910(2), c = 17.636(3) Å, β = 103.220(2)°, V = 1891.7(5) Å3, Z = 4, R 1 = 0.0693, wR 2 = 0.1691. The Mo atom in the complex is octahedrally coordinated, with the tridentate ONO ligand occupying the meridional sites. Thermal stability analysis was performed. The complex shows high catalytic property for the oxidation of various olefins.  相似文献   

20.
A trinuclear copper(II) complex [Cu3Cl2L2], where L is the dianionic form of N,N′-bis(4-methoxysalicylidene)-1,3-pentanediamine, has been synthesized and characterized by means of spectroscopic methods and single crystal X-ray structure determination. The complex crystallizes in the orthorhombic space group Pnma with unit cell dimensions a = 15.301(2), b = 23.226(2), c = 12.089(1)Å, V = 4296.2(8) Å3, Z = 4, R 1 = 0.0682, and wR 2 = 0.1590. The molecule of the complex possesses a crystallographic mirror plane symmetry with the mirror plane passes through the three Cu atoms and the two Cl atoms. The two terminal Cu atoms adopt distorted square pyramidal coordination, and the middle one adopts square planar coordination. The intramolecular Cu…Cu distances are 2.900(1) and 2.916(1) Å. The complex was tested for its antibacterial activity to assess its inhibiting potential.  相似文献   

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