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1.
The 2,11-dithia[3.3](3,5)pyrdinophane (L1) has been synthesized by a new method and characterized by 1H NMR, which is used to form coordination complexes C14H14N4O6S2Ni (I) by addition of Ni2+ cation and C14H14N3O3S2Ag (II) by addition of Ag+ cation. 2,11,20-Trithia[3.3.3](3,5)pyridinophane (L2) and 2,11,20,29-tetrathia[3.3.3.3](3,5)pyridinophane (L3) have also been synthesized as by-products. Single-crystal X-ray analysis reveals that the conformation of the L1 is syn(boat-chair), complexes I and II also adopt syn(boat-chair) (CIF files CCDC nos. 1400332 (I) and 700724 (II)). While in I, Ni(II) is coordinated with L1 with two nitrogen and four oxygen atoms, in II, Ag(I) is coordinated with L1 by two nitrogen and two sulfur atoms came from four ligands. In complexes I and II, the formation of three-dimensional structure depends on π???π stacking and hydrogen bonds.  相似文献   

2.
By self-assembly of delocalized organic ligands (L1 and L2) with Cd(SCN)2, ZnI2 and Zn(NCS)2, three luminescent complexes ZnI2(L1)2 (I), [Cd(L1)21,3-SCN)2] n (II) and Zn(NCS)2(L2)2 (III) were obtained (L1 = 2-{5,5-dimethyl-3-[2-(pyridine-4-yl)ethenyl]cyclohex-2-enylidene}propanedinitrile and L2 = 2-{5,5-dimethyl-3-[2-(pyridine-3-yl)ethenyl]cyclohex-2-enylidene}propanedinitrile). The structures of the complexes were determined by single crystal X-ray diffraction analysis (CIF files CCDC nos. 1406116 (I), 1406115 (II), and 1400360 (III)). In complex I, Zn(II) is coordinated by two functional organic ligands and two I ions, to form a I2N2 distorted tetrahedral geometry. In 1D coordination polymer II, the Cd(II) centers show six-coordinated geometries, two organic ligands and four SCN ions involve in coordination with each Cd(II) center. The thiocyanate groups show μ1,3-SCN bridging coordination modes and the adjacent Cd(II) ions are bridged by double μ1,3-SCN ions to form an infinite chain. In complex III, Zn(II) is coordinated by two functional organic ligands and two NCS groups, to form a N4 distorted tetrahedral geometry. Compared with the free ligands, the complexes show superior luminescent property with red-shift and enhancement of fluorescence intensity.  相似文献   

3.
Hydrothermal reaction of Co(II) salt with 1,4-di(1-imidazolyl)benzene (L1) and 4,4’-oxydiphthalic acid (H4OA) yields a new complex [Co3(HOA)2(L1)4(H2O)4] (I). [Ni(L2)2SO4] · 0.5H2O (II) can be obtained via the hydrothermal reaction of NiSO4 · 6H2O with 1,3-di(1H-imidazol-4-yl)benzene (L2). Complexes I and II have been characterized by single-crystal and powder X-ray diffraction (CIF files CCDC nos. 1019291 (I) and 1019292 (II)), IR, elemental, and thermogravimetric analyses. Complex I exhibits the uninodal six-connected 3D pcu framework structure of I with (412 · 63) topology; Complex II consists of the uninodal four-connected 2D sql (44 · 62) networks. In addition, magnetic property of I was investigated.  相似文献   

4.
Complexes [CuL1Cl2] (I), [CuL2Cl2] · EtOH (II), and Cu2L3Cl4 (III) containing esters of the N-derivatives of optically active amino acids based on (+)-3-carene (L1, L2) and (?)-α-pinene (L3) are synthesized. The crystal and molecular structures of compounds I and II are determined by X-ray diffraction analyses (CIF files CCDC nos. 1560071 (I), 1560072 (II)). The crystal structure of compound I consists of mononuclear complex molecules. In the structure of compound II, the unit cell contains two crystallographically independent molecules of mononuclear complex [CuL2Cl2] and two EtOH molecules. Ligands L1 and L2 perform the tridentate-chelating function by the N atoms of the NH and NOH groups and by the O atom of the C=O group. In compounds I and II, the coordination polyhedra Cl2N2O of the Cu atoms are trigonal bipyramid. According to the data of IR and electronic spectroscopy, binuclear complex III has similar coordination polyhedra. The experimental values of μeff for compounds I, II, and III at 300 K are 1.93, 1.88, and 2.71 μB. For complex III, the μeff(T) dependence in a range of 2–300 K indicates a weak ferromagnetic exchange interaction.  相似文献   

5.
Four new complexes, [Cu2(Bpca)2(L1)(H2O)2] · 3H2O (I), [Cu2(Bpca)2(L2)(H2O)2] (II), [Cu2(Bpca)2(L3)] · 2H2O (III), [Cu2(Bpca)2(L1)(H2O)] · 2H2O (IV) (Bpca = bis(2-pyridylcarbonyl)amido, H2L1 = glutaric acid, H2L2 = adipic acid, H2L3 = suberic acid, H2L4 = azelaic acid) have been synthesized and characterized by single-crystal X-ray diffraction methods (CIF files CCDC nos. 1432836 (I), 1432835 (II), 817411 (III), and 817412 (IV)), elemental analyses, IR spectra. Structural analyses reveal that compounds I, II, and IV have similar structures [Cu(Bpca)]+ units bridged by dicarboxylate forming dinuclear units, whereas the dinuclear of compound III are edge-shared through two carboxylate oxygen atoms of different suberate anions. Hydrogen bonds are response for the supramolecular assembly of compounds I to IV. The temperature-dependent magnetic property of III was also investigated in the temperature range of 2 to 300 K, and the magnetic behaviour suggests weak antiferromagnetic coupling exchange.  相似文献   

6.
Two new complexes were synthesized, namely, 7: 2 (2.2.2-cryptand)potassium chloride and (2.2.2-cryptand)ammonium bromide(0.75)chloride(0.25) hydrates: [M(Crypt-222)]+ · Hal? · 3.5H2O, where M = K, Hal = Cl (I) and M = NH4, Hal = Br0.75Cl0.25 (II). The structures of two isomorphous crystals were studied by X-ray diffraction analysis. Trigonal (space group P \(\bar 3\), Z = 2) structures I (a = 11.763 Å, c = 11.262 Å) and II (a = 11.945 Å, c = 11.337 Å) were solved by direct methods and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.057 (I) and 0.065 (II) for all 2626 (I) and 1654 (II) independent measured reflections (CAD-4 automated diffractometer, λMoK α). In structures I and II, the host-guest [M(Crypt-222)]+ complex cation lies on the threefold crystallographic axis and has the approximate D 3 symmetry. In complex I, the coordination polyhedron of the K+ cation (CN = 8) is a bicapped trigonal prism somewhat distorted toward an antiprism. Complexes I and II contain H-bonded disordered cubes of the water molecules and the Cl? or Br? anions.  相似文献   

7.
The syntheses of a mononuclear zinc(II) complex [ZnCl(L1)(Amp)] (I) and a mononuclear nickel(II) complex [Ni(L2)(HL2)](BF4) · 0.5H2O (II) (HL1 = 4-methyl-2-[(4-methylpyridin-2-ylimino) methyl]phenol, HL2 = 4-methyl-2-[(pyridin-2-ylmethylimino)methyl]phenol; Amp = 2-amino-4- methylpyridine) were prepared under microwave irradiation. The complexes were characterized by a combination of elemental analyses, and IR and electronic spectra. Their structures were further confirmed by single crystal X-ray crystallography (СIF files CCDC nos 1437737 (I), 1437738 (II)). The Zn atom in the monomeric complex I is in tetrahedral coordination. The Ni atoms in the dimeric complex II are in octahedral coordination. Crystals of the complexes are stabilized by hydrogen bonds. In order to evaluate the biological activity of the complexes, in vitro antibacterial against Staphylococcus aureus, Bacillus subtilis, Escherichia coli, and Pseudomonas aeruginosa was assayed. The complexes have strong activity against Bacillus subtilis.  相似文献   

8.
Two complexes, (2.2.2-cryptand)rubidium chloride and bromide hydrates [Rb(Crypt-222]Hal · 3.5H2O (Hal = Cl (I) and Br (II)), are synthesized. The structures of isomorphic crystals of compounds I and II are studied by X-ray diffraction analysis. The crystals are trigonal: space group P \(\overline 3 \), Z = 2; I: a = 11.810 Å, c = 11.302 Å; II: a = 11.890 Å, c = 11.402 Å. The structures are solved by a direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.060 (I) and 0.077 (II) for 2650 (I) and 2700 (II) independent reflections (CAD-4 automated diffractometer, λMoK α radiation). In crystals of complexes I and II, the [Rb(Crypt-222)]+ cation of the host-guest type lies on the crystallographic axis 3 and has the approximate symmetry D 3. In complexes I and II, the coordination polyhedron of the Rb+ cation is a two-base-centered trigonal prism somewhat distorted to an antiprism. The crystals of compounds I and II contain H-bonded disordered cubes of the water molecules and Cl? or Br? anions.  相似文献   

9.
Zinc(II) and manganese(II) complexes of 2-(diphenylacetyl)indandione-1,3 (HL) were synthesized. Crystals of [M(DMSO)2L2] · CHCl3, where M= Zn(II) (I) and Mn(II) (II), obtained from chloroform plus dimethyl sulfoxide (DMSO) mixture were found to be isostructural based on the similarity of their unit cell parameters and unit cell volumes. The crystals are triclinic, Z = 2, space group P \(\bar 1\); a = 10.422(1) Å, b = 11.929(1) Å, c = 20.429(1) Å, α = 73.616(1)°, β = 85.095(1)°, γ = 77.586(1)° for complex I; a = 10.436(1) Å, b = 12.297(1) Å, c = 19.924(2) Å, α = 78.138(2)°, β = 87.625(2)°, γ = 82.048(2)° for complex II. X-ray structural analysis of complex I was carried out. For complex II, the structure was not refined because all of its atoms are each disordered over three to five positions. The two DMSO molecules in complex I coordinate the central metal atoms in the monodentate mode via their donor oxygen atoms to occupy an axial position and an equatorial position in an octahedral polyhedron. The other four positions are occupied by the four oxygen atoms of the two deprotonated ligands L? coordinated in the bidentate-cyclic mode. The outer sphere of complex I contains the solvating chloroform molecule.  相似文献   

10.
The NiCl2 and CoCl2 complexes with 4,5-(2-pyridylethylene)-dithio-1,3-dithiol-2-thione (L1) and 4,5-(4-pyridylethylene)-dithio-1,3-dithiol-2-thione (L2) were described. The L1 ligand shows bidentate coordination through the pyridyl N atoms and the thiol S atoms in a tetrahedral [CoCl2(L1)] complex (I) and in an octahedral [NiCl2(L1)2](MeCN)2 complex (II). The L2 ligand exhibits monodentate coordination through the pyridyl N atom in tetrahedral complexes [CoCl2(L2)2 (III) and [NiCl2(L2)2] (IV). Complexes I, III, IV in crystal state are octahedral due to extra coordination of the thione S atoms or the chloride bridges responsible for the polymeric structure. The structure of the complex II · CH2Cl2 was determined by X-ray diffraction analysis. The crystals are monoclinic, space group P21/c, a = 11.895(2) Å, b = 13.374(3) Å, c = 21.873(4) Å, β = 95.30(3)°, Z = 2. The Ni atom has quasi-tetrahedral surrounding due to two chloride ions and two L1 ligands coordinated through the pyridyl N atoms and the thiol S atoms.  相似文献   

11.
Two Co(III) dioximates, cyanoguanidine complex {[Na2(µ-H2O)2(L1)2(H2O)2]-[CoIII(DmgH)2(N3)2]} n [CoIII(DmgH)2(N3)2] n (L1 = (H2N)2C=N–C=N) (I) and aminoguanidine complex [H3L2][Co(DmgH)2(N3)2] (H2L2 = H2N–C(=NH)–NH–NH2) (II), were synthesized from the [CoCl(DmgH)2(H2O)] structural unit (DmgH is the dimethylglyoxime monoanion). The implementation of the synthesis was confirmed by chemical analysis, IR spectroscopy, and X-ray diffraction (CIF files CCDC 1531845 (I), 1531846 (II)). Both compounds are ionic. Compound I consists of cations representing centrosymmetrical 2D coordination polymers, {[Na2(µ-H2O)2(L1)2(H2O)2][CoIII(DmgH)2(N3)2]} n+ n , and monomeric [Co(DmgH)2(N3)2] anions, while in II, the charge of the [Co(DmgH)2(N3)2] complex anion is counterbalanced by the organic [H3L2]+ cation. In I, L1 is coordinated to the metal as a monodentate neutral ligand, while in II, H2L2 occurs in the complex as a protonated uncoordinated component. Since L1 in I and H2L2 in II contain functional amine groups able to form intermolecular hydrogen bonds acting as proton donors, the component packing mode in the crystals was analyzed assuming various types of interactions, apart from electrostatic ones. The biological properties of the complexes were tested considering their effect on the biosynthesis of proteases by the micromycete Fusarium gibbosum CNMN FD 12 strain. Culturing the producer on a culture medium containing complex I in the selected optimal concentrations of 5–10 mg/L was found to increase the acid protease activity by 140–150%.  相似文献   

12.
The phenolic azide bridged dinuclear nickel(II) complex, [Ni2(L1)2(N3)(H2O)(μ1,1-N3)] · EtOH (I), and the thiocyanate bridged dinuclear copper(II) complex, [Cu2(L2)21,1-NCS)2] (II), where L1 and L2 are the deprotonated forms of 2-mothoxy-6-[(2-piperidin-1-ylethylimino)methyl]phenol and 2,4-dichloro-6-[(2-methylaminoethylimino)methyl]phenol, respectively, were synthesized and characterized by elemental analysis, IR spectra, and single-crystal X-ray diffraction. The crystal of I is orthorhombic: space group Pbca, a = 12.172(1), b = 20.953(1), c = 29.779(2) Å, V = 7594.8(9) Å3, Z = 8. The crystal of II is monoclinic: space group P21/n, a = 8.7615(11), b = 19.672(2), c = 16.568(2) Å, β = 99.449(2)°, V = 2816.9(6) Å3, Z = 4. The Ni atoms in I are in octahedral coordinations, and the Cu atoms in II are in square-pyramidal coordinations.  相似文献   

13.
Different-metal different-ligand complexes [{Co(Phen)3}2{Co(Phen)(H2O)4}2][{Ge(μ-OH)(μ- Hedp)}6Cl2] (I), [{Cu(Phen)2(H2O)}2(HPhen)2][Ge(μ-OH)(μ-Hedp)]6 · 20H2O (II) (H4Hedp = 1-hydroxyethylidenediphosphonic acid, Phen = 1,10-phenanthroline) were synthesized and studied by X-ray diffraction. According to X-ray diffraction data (CIF files CCDC nos. 1573112 (I), 1573113 (II)), compounds I and II are cation–anion type complexes in which the anions are represented by {[Ge(μ-OH)(μ-Hedp)]6}6– and, in the case of I, two additional Cl ions, while the cations are [Co(Phen)3]2+, [Co(Phen)(H2O)4]2+ in I and [Cu(Phen)2(H2O)]2+, HPhen+ in II. In the crystals of compounds I and II, the cations, anions, and water molecules are combined by numerous intermolecular hydrogen bonds, giving rise to a 3D network.  相似文献   

14.
An end-on azido-bridged dinuclear nickel(II) complex [Ni2(L1)21,1-N3)2] · CH3COOH (I) and an end-on azido-bridged polynuclear copper(II) complex [CuL21,1-N3)] n , where L1 is the deprotonated form of 2-[(2-ethylaminoethylimino)methyl]-4-fluorophenol and L2 is the deprotonated form of 2-[(2- dimethylaminoethylimino)methyl]-4-fluorophenol, were prepared and characterized by elemental analysis and FT-IR spectra. Crystal and molecular structures of the complexes were determined by single crystal X-ray diffraction method (CIF files CCDC nos. 942641 (I) and 942642 (II)). Single crystal X-ray structural studies indicate that the Schiff base ligands coordinate to the metal atoms through phenolate oxygen, imine nitrogen, and amine nitrogen. The Ni atoms in the nickel complex are in octahedral coordination, and the Cu atoms in the copper complex are in square pyramidal coordination. Crystals of the complexes are stabilized by hydrogen bonds. The Schiff bases and the complexes showed potent antibacterial activities.  相似文献   

15.
Two copper complexes with long rigid ligands, Cu(Tta)2(L1) (I), and Cu(Tta)2(L2) (II), where L1 = (E)-3-(4-(1H-benzo[d]imidazol-1-yl)-(4-phenyl)phenyl)-1-phenylprop-2-en-1-one, L2 = (E)-3-(4-(1H-imidazol-1-yl)phenyl)-1-(4-phenyl)phenyl)prop-2-en-1-one), have been synthesized and characterized. The single-crystal X-ray analysis (CIF files CCDC nos. 1409671 (I) and 1409672 (II)) for complexes I and II demonstrates that each copper ion assumes a distorted square-pyramidal MO4N polyhedron in which four oxygen atoms come from the Tta ligands, and one nitrogen atom comes from the N-donor ligand. Both of the complexes are linked into 3D networks through weak intermolecular interactions.  相似文献   

16.
Two crystalline host-guest complexes are synthesized and studied using X-ray diffraction analysis: (18-crown-6)sodium tribromide [Na(18-crown-6)]+ · Br 3 ? (I) and (18-crown-6)potassium tribromide (with an admixture of bromodiiodide) [K(18-crown-6)]+ · (Br0.25I2.75)? (II). The structures of compound I (space group P21/n, a = 8.957 Å, b = 8.288 Å, c = 14.054 Å, β = 104.80°, Z = 2) and compound II (space group Cc, a = 8.417 Å, b = 15.147 Å, c = 17.445 Å, β = 99.01°, Z = 4) are solved by a direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.098 (I) and 0.036 (II) for all 2311 (I) and 2678 (II) independent measured reflections on a CAD-4 automated diffractometer (λMoK α). Similar crystalline complexes I and II exist as infinite chains of alternating complex cations and trihalide anions linked to each other through weak Na-Br or K-I coordination bonds. In [Na(18-crown-6)]+ and [K(18-crown-6)]+ complex cations, the Na+ or K+ cation (coordination number is eight) is located in the center of the cavity of the 18-crown-6 ligand and coordinated by the six O atoms and two terminal Br or I atoms of two trihalide anions lying on opposite sides of the rms plane of the crown ligand.  相似文献   

17.
Heteroligand complexes [Co2(HMTA)(iso-Bu2PS2)4] (I) (μeff = 4.67 μB) and [Cd2(HMTA)(iso-Bu2PS2)4] (II) have been synthesized. Single crystals of compounds I and II have been obtained. The crystals are monoclinic: a = 32.622(2) Å, b = 9.4891(6) Å, c = 21.7570(13) Å, β = 125.774(1)o, V = 5464.3(6) Å,3, Z = 4, ρcalcd = 1.331 g/cm3 for I; a = 34.6092(7) Å, b = 9.5595(2) Å, c = 22.3473(5) Å, β = 127.144(1)o, V = 5893.5(2) Å, Z = 4, ρcalcd = 1.355 g/cm3 for II; space group for both complexes C2/c. Structures I and II are based on discrete binuclear molecules. The coordination polyhedra of the Co and Cd atoms are distorted tetragonal pyramids NS4, with the bases formed by four S atoms of two bidentate chelating ligand iso-Bu2PS 2 ? and the axial vertices occupied by N atoms of bidentate bridging HMTA ligand. The character of interaction of the molecules in structures I and II is considered.  相似文献   

18.
A reaction between VOSO4, 2,6-diacetylpyridine, and nicotinohydrazide in a molar ratio of 1: 1: 2 afforded two complexes differing in both color and crystal shape as well as in chemical composition and molecular structure. The compositions and structures of the vanadium complexes were determined by IR spectroscopy and X-ray diffraction (CIF files CCDCnos. 1411235 (I) and 1411236 (II)). These complexes can be formulated as [V 2 II (H2L)2](NO3)4 ? H2O (I) and [VIV(=O)(H2L)(SO4)] ? 5H2O (II), where H2L is 2,6-diacetylpyridine bis(nicotinylhydrazone). Complex I consists of centrosymmetric dinuclear complex cations [V2(H2L)2]4+, NO 3 - anions, and crystal water molecules in a ratio of 1: 4: 1; complex II is built from molecular V(IV) complexes and crystal water molecules in a ratio of 1: 5. The coordination polyhedron of the metal atom in I is a tetragonal pyramid made up of the electron-donating atoms N3O2 of two ligands H2L. The coordination polyhedron of the metal atom in II is a pentagonal bipyramid made up of the electron-donating atoms N3O2 of one neutral five-coordinate ligand H2L and two O atoms coming from the oxo ligand and the SO 4 2- anion coordinated in a monodentate fashion.  相似文献   

19.
A new cobalt(II,III) complex, [CoIIIL2]2[Co 2 II (HL)2(OH2)2(CH3OH)2] ? 2H2O (I) and a new iron(III) complex, [FeIII(HL)2](NO3) (II), where L2– and HL are the dianionic and monoanionic form of N'-(2-hydroxybenzylidene)-3-methylbenzohydrazide, respectively, have been prepared and characterized by elemental analyses, infrared and UV-Vis spectroscopy and single-cyrstal X-ray diffraction (CIF files CCDC nos. 1417971 (I), 1417979 (II)). Complex I crystallizes in the monoclinic space group P21/n with unit cell dimensions a = 16.1665(9), b = 14.5692(8), c = 19.086(1) Å, β = 96.347(1)°, V = 4467.9(4) Å3, Z = 2, R 1 = 0.0521, and wR 2 = 0.1411. Complex II crystallizes in the orthorhombic space group Pbcn with unit cell dimensions a = 12.475(1), b = 12.202(1), c = 18.859(2) Å, V = 2870.8(4) Å3, Z = 4, R 1 = 0.0796, and wR 2 = 0.1981. The metal atoms in the complexes are in octahedral coordination. Crystals of the complexes are stabilized by hydrogen bonds. The efficiency of the aroylhydrazone and the two complexes was evaluated against B. subtilis, S. aureus, E. coli, P. fluorescence, C. albicans and A. niger, with the complexes demonstrating enhanced activity relatively to the free ligand.  相似文献   

20.
Two new cobalt(III) and zinc(II) complexes, [Co(L1)2 (H2O)] · ClO4 (I) and [Ni(L2)2 (H2O)2] · 2ClO4 (II), where L1 is the deprotonated form of 5-methoxy-2-[(2-morpholin-4-ylethylimino)methyl]phenol, and L2 is the zwitterionic form of 2-[(2-isopropylaminoethylimino)methyl]-5-methoxyphenol, were synthesized and structurally characterized by elemental analyses, IR spectra, and single-crystal X-ray diffraction. The crystal of I is monoclinic: space group P21/c, a = 11.1512(4), b = 28.2424(11), c = 10.9655(4) Å, β = 95.746(2)°, V = 3436.1(2) Å3, Z = 4. The crystal of II is triclinic: space group P21/c, a = 8.1441(2), b = 10.4531(3), c = 10.8849(3) Å, α = 84.0240(10)°, β = 76.9800(10)°, γ = 74.2280(10)°, V = 867.92(4) Å3, Z = 1. Complex I consists of a mononuclear cobalt(III) complex cation and a perchlorate anion. Complex II consists of a crystallographic centrosymmetric mononuclear nickel(II) complex cation and two perchlorate anions. Each metal atom in the complexes is in an octahedral coordination.  相似文献   

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