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1.
A new complex [Cu(phen)3][(C6H5)2C(OH)COO]2·6H2O was prepared by self-assembly of benzilic acid, 1,10-phenanthroline (phen), and copper perchlorate. It crystallizes in triclinic, space group P1, with a = 1.14661(17), b = 1.6455(2), c = 1.6457(2) nm, α = 74.779(2), β = 74.904(3), γ = 84.424(3)o, V = 2.8914(7) nm3, Dc = 1.340 g/cm3, Z = 2, F(000) = 1218, GOOF = 1.018, the final R = 0.0643 and wR = 0.1633. The crystal structure shows that the copper ion is coordinated with six nitrogen atoms from six 1,10-phenanthroline molecules, forming a distorted octahedral coordination geometry.  相似文献   

2.
A new cadmium complex [Cd(phen)3]·(ClO4)2·(α-FRA)-(H2O)3 was prepared by self-assembly of α-furoic acid, 1,10-phenanthroline (phen), and cadmium perchlorate. It crystallizes in the monoclinic system, space group P21/n, with a = 1.28130(15), b = 2.5957(3), c = 1.35449(16) nm, β = 109.395(2)°, V = 4.2492(9) nm^3, Dc = 1.491 g/cm^3, Z = 4, F(000) = 1926, GOOF = 1.023, the final R = 0.0729 and wR = 0.2086. The crystal structure analysis indicates that the cadmium ion is coordinated with six nitrogen atoms from six 1,10-phenanthroline molecules, giving a distorted octahedral coordination geometry. The cyclic voltametric behavior of the complex was also investigated.  相似文献   

3.
One novel complex [Ni(phen)3],(C8H12O4)·(H2O)14 with hexane dicarboxylic acid and 1,10-phenanthroline has been hydrothermally synthesized and characterized. Crystal data: monoclinic, space group C2/c, a = 2.3475(5), b = 1.2208(2), c = 1.9499(4) nm, β= 114.682(3)°, V = 5.0778(16) nm^3, Dc = 1.339 g/cm^3, Z = 4,μ(MoKa) = 0.458 mm^-1, F(000) = 2168, GOOF = 1.014, R = 0.0401 and wR = 0.0961. The nickel(H) center in the title complex is coordinated with six nitrogen atoms of three 1,10-phenanthroline molecules, giving a distorted octahedral coordination geometry. However, the nickel(Ⅱ) ion does not coordinate to the hexane dicarboxylic acid. The complex molecules form a 3D structure through hydrogen bonds. TG analysis shows that the title complex is stable below 240.0 ℃.  相似文献   

4.
The title complex, [Ce(BA)3phen]2 (BA = benzoate, phen = 1,10-phenanthroline), was prepared by the reaction of Ce(NO3)3.6H2O, benzoic acid and 1,10-phenanthroline. The complex was characterized by single-crystal X-ray diffraction, elemental analysis, IR spectra and TG-DTG techniques. The results show that the crystal is of triclinic, space group P1 with a = 10.912(2), b = 11.962(3), c = 12.474(3) A, α = 104.889(3), β = 93.523(3), γ = 113.332(3)^o, C66H46Ce2N4O12, Mr = 1366.90, V= 1420.2(6) ,A^3, Z = 1, Dc = 1.598 g/cm^3, μ = 1.652 mm^-1, S = 1.024 and F(000) = 682. The final R = 0.0391 and wR = 0.0947 for 4878 observed reflections with I 〉 2σ(I). The structure of the title complex consists of two Ce(C6HsCOO)3(C12H8N2) units, forming a binuclear molecule. Each Ce(Ⅲ) is coordinated by two O atoms of one bidentate chelating carboxylate group, five O atoms of two bidentate bridging and two tridentate chelating-bridging carboxylate groups, and two N atoms of one 1,10-phenanthroline molecule to complete a distorted monocapped square antiprism geometry. Its thermogravimetric analysis was determined by TG-DTG techniques.  相似文献   

5.
李薇  李昶红  杨颖群  匡云飞 《结构化学》2007,26(10):1228-1231
The title complex (C26H18CuN2O6,Mr=517.96) has been synthesized by the reac-tion of α-furanacrylic acid with 1,10-phenanthroline (phen) in the solvent mixture of water and methanol. Crystal data: monoclinic,space group C2/c with a =2.2927(4),b=1.01248(18),c=1.05061(18) nm,β=111.188(3)o,V=2.274(7) nm3,Dc=1.513 g/cm3,Z=4,F(000)=1060,μ= 1.007mm?1,R=0.0320 and wR=0.0781. The crystal structural analysis shows that the copper atom is coordinated with four oxygen atoms from two α-furacrylic acids and two nitrogen atoms from 1,10-phenanthroline,giving a distorted octahedral coordination geometry. The result of electroche-mical analysis shows that the electron transfer in the electrode reaction is quasi-reversible.  相似文献   

6.
A mixed-ligand metal-organic complex [Cd(C7H3N3O2)(C12H8N2)]n was synthesized by cadmium(Ⅱ) nitrate, 1,10-phenanthroline(phen) and benzotriazole-5-carboxylate acid(H2btca). Single crystal X-ray analysis indicates that complex 1 has a two-dimensional layer structure and crystallizes in an orthorhombic space group(Pbca), with cell parameters, a=1.7422(6) nm, b=0.9264(3) nm, c=2.0729(7) nm, α=90°, β=90°,γ=90°, V=3.346(2) nm^3, Z=8. Each central Cd(Ⅱ) is six-coordinated by four N atoms, two of which are from 1,10-phenanthroline, and the other two from two different triazole nitrogen atoms and two O atoms from benzotriazole-5-carboxylate, forming a distorted octahedral geometry. Adjacent Cd(Ⅱ) centers are bridged by benzotriazole-5-carboxylate molecules to form a one-dimensional chain, which is further connected by the nitrogen atoms of btca^2- to form an extended two-dimensional wave-like layer, with OFF(offset face-to-face) stacking interactions between phen ligands in adjacent layers, which are helpful to forming the three-dimensional supramolecular structure.  相似文献   

7.
范赛荣  朱龙观 《中国化学》2005,23(10):1292-1296
Cobait(Ⅱ) nitrate reacted with 1,10-phenanthroline (phen) and 5-sulfosaiicylic acid (H3ssal) to yield the cobait(Ⅰ) complex [Co(phen)2(H2O)2](Hssal)o4H2O (1) and the reaction of 1 with copper acetate led to a novel complex [Co(phen)(H2O)4][Cu2(ssal)2(phen)2]·5H2O (2). These two complexes were cationanion species and the cationic motif [Co(phen)2(H2O)2]^2+of 1 could be converted to [Co(phen)(H2O)4]^2+ in the formation process of new anion [Cu2(phen)2(ssal)2]^2- of 2. In both complexes abundant hydrogen bonds construct different supramolecular architectures, thus the conversion reaction can provide a new path to create novel supramolecular network.  相似文献   

8.
张少华  李昶红  李薇  谭雄文  周水奇 《结构化学》2011,30(10):1493-1496
The title complex has been synthesized with 2,2'-biphenyl dicarboxylic acid and 1,10-phenanthroline(phen)in the solvent mixture of water and methanol.It crystallizes(C38H28CuN4O6,Mr = 700.1)in triclinic,space group P1 with a = 1.0868(2),b = 1.2175(2),c = 1.6206(3)nm,α = 110.161(2),β = 102.605(3),γ = 93.667(2)o,V = 1941.6(6)nm3,Dc = 1.198 g/cm3,Z = 2,F(000)= 722,R = 0.0558 and wR = 0.1208.The crystal structure shows that the copper atom is coordinated with one oxygen atom from 2,2'-bphenyl dicarboxylic acid molecule and four nitrogen atoms from two 1,10-phenanthroline molecules,forming a distorted square-pyramidal coordination.The TG analysis shows that the title complex is stable under 160.0 ℃.  相似文献   

9.
A new dinuclear La(Ⅲ) complex [La2(4-cba)4[H(4-cba)2]2(phen)2(H2O)4] (4-Hcba = 4-cyanobenzoic acid and phen = 1,10-phenanthroline) 1 has been synthesized by solvothermal reaction in an ethanol/water mixed solution at 100 ℃ and structurally characterized by singlecrystal X-ray diffraction. Crystallographic data: C88H58La2N12O20, Mr = 1881.28, triclinic P1, a = 7.518(3), b = 17.033(6), c = 17.551(6)A, α = 115.333(4), β = 92.9910(10), γ = 99.366(5)°, V = 1985.3(12)A^3, Z = 1, Dc = 1.574 g/cm^3, F(000) = 944 μ = 1.145 mm^–1, the final R = 0.0281 and wR = 0.0686 for 6708 reflections with Ⅰ 〉 2σ(I). In 1, two nine-coordinated La(Ⅲ) ions are connected by two 4-cba ligands in a syn-syn bidentate coordination mode, and the other six 4-cba ligands terminate the La(Ⅲ) ions, resulting in an isolated dinuclear structure. Two different types of intramolecular hydrogen bonds, asymmetrical O-H…O and symmetrical O…H…O, exist in the crystal. The title complex molecules are connected through hydrogen bonds and weak π-π stacking interactions to generate a 2-D layered network. The thermogravimetric analysis of 1 has also been discussed.  相似文献   

10.
A supramolecular framework, 1.5Zn(phen)3·L·3NO3 (C63H48Zn1.5N16O9S), has been synthesized. The ligand L was synthesized by the condensation of p-aminoacetophenone with thiosemicarbazide. The crystal belongs to the monoclinic system, space group C2/c, with a = 31.005(2), b = 15.114(2), c = 24.887(3) A, β = 94.260(2)° Z = 8, V = 11630(2)A^3 Dc = 1.489 g/cm^3, Mr = 1303.29,λ(MoKa) = 0.71069 A,μ= 0.735 mm^-1, F(000) = 5368, Rint = 0.0699, R= 0.0505 and wR= 0.0707. Two independent Zn atoms are both coordinated by six N atoms from three phen ligands. π-π and C-H…π interactions among the L ligands and Zn(phen)3 cations, π-π and C-H...π interactions among the Zn(phen)3 cations and N-H...O hydrogen bonds among the L ligands and nitrate anions connect the whole structure into a 3-D supramolecular framework.  相似文献   

11.
A new ternary copper(II) complex,[C 43 H 27 Cu 2 N 7 O 5 ]·[C 14 H 6 CuN 2 O 8 ]·6.5H 2 O,has been synthesized by the reaction of copper sulfate,2,6-pyridinedicarboxylic acid and 1,10-phenanthroline (phen),and characterized by elemental analysis,IR,UV and X-ray single-crystal diffraction.It crystallizes in triclinic,space group P1,with a=14.379(5),b=15.510(5),c=15.835(6),α=78.567(6),β=63.594(6),γ=81.287(6)°,V=3092.1(19)3,C 57 H 46 Cu 3 N 9 O 19.5,M r=1359.54,Z=2,D c=1.446 Mg/m 3,λ(MoKα)=0.71073,μ=1.101 mm-1,F(000)=1362,S=1.071,the final R=0.0718 and wR=0.11960 for 10705 observer reflections (I > 2σ(I)).The structure unit of the title complex consists of a mononuclear part and a di-nuclear part,and the three copper ions show three coordination modes.Each 6-coordinated geometry of the Cu atom is a distorted octahedral coordination geometry.The 3D supramolecular system is formed by the hydrogen bond O-H···O and π-π stacking interaction between neighboring single cells.The antibacterial activity of the title complex is also studied.  相似文献   

12.
许金生  袁亚莉 《结构化学》2009,28(10):1325-1328
One new cobalt complex [Co(phen)3][(C6Hs)2C(OH)COO]2·7H2O with benzeneacetic acid (BAA), 1,10-phenanthroline and cobaltous perchlorate has been synthesized by means of solvent method. It crystallizes in the triclinic system, space group P^-1, with a = 1.14181(13), b = 1.64417(18), c = 1.65342(18) nm, α = 74.2830(10), β= 84.4490(10), γ = 74.9430(10)°, V = 2.8842(6) nm^3, Dc = 1.359 g/cm^3, Z = 2, F(000) = 1234, R = 0.0621 and wR = 0.1673. The crystal structure shows that the cobalt ion is coordinated with six nitrogen atoms from three 1,10-phenanthroline molecules, giving a distorted octahedral coordination geometry. There are a lot of hydrogen bonds in the complex, from which a two-dimensional network is constructed. The result of TG analysis shows that the title complex is stable below 130.0 ℃.  相似文献   

13.
At room temperature, dibenzoyl peroxide undergoes oxidative addition reaction with metallic copper powder and pyridine N-oxide (triphenylphosphine oxide or 2,9-dimethyl-4,7-diphenyl-1,10-phenanthrolin) which affords the last products as binuclear copper(II) complexes, [Cu(C5H5NO)-(C6H5COO)2]2(1), [Cu(OPPh3)(C6H5COO)2]2(2) and [Cu(C6H5COO)(C26H2oN2)](3, C26H2oN2 is 2,9-dimethyl-4,7-diphenyl-1,10-phenanthrolin). The structure of the complexes were characterized by elemental analyses, IR spectra, TG-DTA and magnetic property. Crystals(1) are triclinic, space group P1,a=0.92617(36),b=1.06973(17), c=1.08813(29) nm, a=59.60(2)°, β=74.83(3)°,γ=72.80(2)°, V=0.880 nm3, Dc=1.520 g/cm3, Z=1, R=0.044, Rw=0.048, Mr=805.78, 3477 reflections with I > 3σ(I). Each copper(Ⅱ) ion is coordinated by two bridging bidentate benzoate ligands and one pyridine N-oxide or triphenylphosphine oxide to form dimeric binuclear molecules. The structure of the compound(1) shows a clear centre of symmetry.  相似文献   

14.
The two title compounds [Cu(sdba)(py)2(H2O)]n·2n(py) 1 and [Cu(sdba)(phen)(H2O)]n 2 (H2sdba = 4,4′-sulfonyldibenzoic acid, py = pyridine, phen = 1,10-phenanthroline) have been synthesized and characterized by single-crystal structure determination, IR and TG analyses. Compound 1 crystallizes in orthorhombic, space group Pbcm with a = 5.9833(12), b = 22.333(5), c = 24.571(5)A, V = 3283.3(12) A^3, Z = 4, C34H30N4OTSCu, Mr = 702.22, Dc = 1.388 g/cm^3, F(000) = 1396,μ(MoKa) = 0.780 mm^-1, the final R = 0.0599 and wR = 0.1767 for 3416 observed reflections with I 〉 2σ(I). Compound 2 crystallizes in monoclinic, space group C2/c with a = 22.9549(4), b = 12.2443(3), c = 17.8687(4)A, β = 110.873(1)°, V = 4692.69(18)A^3, Z = 8, C26H18N2O7SCu, Mr = 566.02, Dc = 1.602 g/cm^3, F(000) = 2312,μ(MoKa) = 1.078 mm^-1, the final R =0.0697 and wR = 0.1330 for 3452 observed reflections with I 〉 2σ(I). In both structures, the Cu^Ⅱ metal centers adopt five-coordination in slightly distorted tetragonal pyramidal geometries, while the second N-donor ligands bond or chelate to Cun ions as the terminal moiety. The weak interactions extend the two structures into high-dimensional supramolecular coordination-polymers.  相似文献   

15.
A new metal-organic complex Mn2(cbba)4(phen)2 (Hcbba = 2-(4'-chlorine-benzoyl)- benzoic acid, phen = 1,10-phenanthroline) 1 has been hydrotherrnally synthesized and structurally characterized by single-crystal X-ray diffraction, elemental analyses and IR spectroscopy. The compound crystallizes in orthorhombic, space group Pbcn with α = 12.154(5), b = 18.166(7), c = 31.197(13) A, V = 6887(5) A^3, C80H48Cl4Mn2N4O12, Mr= 1508.90, Dc = 1.455 g/cm^3, μ(MoKα) = 0.591 mm^-1, F(000) = 3080, Z = 4, the final R = 0.0408 and wR = 0.0873 for 4033 observed reflections (I 〉 2σ(I)). In the crystal structure, the manganese atom is six-coordinated with four carboxylate oxygen atoms from three different cbba ligands and two nitrogen atoms from phen ligands, showing a distorted octahedral geometry. Furthermore, it exhibits a 3D supramolecular network through π-π interactions.  相似文献   

16.
The copper complex Cu(C12H9N2O3)2 has been synthesized by the reaction of furaldehyde salicylylhydrazone (Hfs) and copper acetylacetonate and characterized by X-ray crystal diffraction and spectroscopic studies. The crystal crystallizes in space group P211n with a = 5.9765(3), b = 15.7196(9), c = 12.0514(6)A,β= 101.618(3)^o, V = 1109.0(1)A^3, C24H18CuN4O6, Mr = 521.96, Z = 2, Dc = 1.563 g/cm^3, μ = 1.035 mm^-1, F(000) = 534, R = 0.0373 and wR = 0.1058 for 2283 observed reflections (I 〉 2σ(I)). The copper atom has a square-planar CuN2O2 coordination and should be in an octahedral coordination if considering Cu-O (phenol) with distances of 2.796(2)A as weak bonds. The neighboring copper complex molecules are linked together by these weak Cu-O (phenol) bonds, resulting in an extended 1D chain. The title compound exhibits paramagnetic property and fluorescence behavior at room temperature supported by the EPR and fluorescence spectra.  相似文献   

17.
A new mononuclear Cu(Ⅱ) dithiocarbamate complex CuI(prdtc)(phen) 1 (prdtc = N-pyrrolidinyldithiocarbamate, phen = 1,10-phenanthroline) was synthesized and characterized by elemental analysis, IR spectrum, and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 8.7110(9), b = 14.7143(14), c = 14.8507(15) A, β = 109.721(6)°, V = 1791.9(3) A3, Z = 4, Dc = 1.916 g/cm3, CI7H16CulN3S2, Mr = 516.89, λ(MoKa) = 0.71073A,μ = 3.178 mm^-1, F(000) = 1012, the final R = 0.0369 and wR = 0.0987. A total of 4082 unique reflections were collected, of which 2916 with I 〉 2σ(I) were observed. The Cu(Ⅱ) atom is five-coordinated in a distorted square-pyramidal geometry by one I atom in the apical position, two S atoms from a prdtc ligand and two N atoms from a phen ligand in the basal plane. There exist face-to-face aromatic π-π stacking interactions between adjacent phen ligands stabilizing the structure and making the complex assemble into a 1D structure along the a axis. It can be concluded that the difference of the dtc flexibility and reaction conditions result in the structural difference between complex 1 and CuI(dmdtc)(phen) (dmdtc = N, N-dimethyldithiocarbamate).  相似文献   

18.
The hydrothermal reaction of copper chloride dihydrate and 5,5-dimethyl-imidazolidine,-2,4-dione with a mole ratio of 1:1 in acetonitrile resulted in the formation of a new acetate-bridged dinuclear copper complex, [C2H6ON]2[Cu2Cl2(μ-CH3COO)4]. Protonated acetamide in eaolie form and acetic acid were yielded by the hydrolysis of acetonitrile under hydrothennal condition. The rifle complex (C12H24Cl2Cu2N2O10) was characterized by X-ray single-crystal diffraction, IR spectrum, elemental and electrochemical analysis. It crystallizes in the monoclinic system, space group P21/c with a = 8.298004), b = 14.358(2), c = 12.0010(2) A^°, β= 130.620(3)°, V = 1085.3(2) A^°^3, Dc = 1.696 g/cm^3, 34, = 554.31, Z = 2, F(000) = 564 and μ = 2.254 mm^-1. The crystal structure consists of a tetraacetate-bridging dinulcear copper complex anion [Cu2Cl2(μ-CH3COO)4]^2-, with the chlorine anions in the axial positions, and two protonated acetamide cations [C2H6ON]^+, which were connected through hydrogen bonds to form a three-dimensional infinite network.  相似文献   

19.
Two manganese complexes, [Mn3(2-cba)6(phen)2] 1 (2-cba = 2-cyanobenzoic acid, phe11 = 1,10-phenanthroline) and [MnE(4-fbaO)E(phen)4](PF6)E.EHEO 2 (4-fbao = 4-formylbenzoic acid oxime), have been synthesized by the reaction of 2-formylbenzoic acid oxime (2-fbao, HELl) or 4-formylbenzoic acid oxime (4-fbao, HELE) with phen and manganese acetate in ethanol or methanol solution. A translation from the oximino (-CHN=OH) of HELl to cyano (-C-N) was found in the formation of complex 1 at room temperature. The complexes were structurally determined by single-crystal X-ray diffraction. The crystal of compound I belongs to monoclinic, space group C2/c, with a = 17.983(6), b = 23.364(7), c =14.589(5) A, β = 92.401(5)° V = 6124(3) A^3, Z = 4, C72H40Mn3N10O12, Mr= 1401.96, Dc = 1.521 g/cm^3, F(000) = 2852.0, Rint = 0.0372, T= 293(2) K,μ = 0.686 mm^-1, the final R = 0.0644 and wR = 0.1813 for 5803 observed reflections with I 〉 2δ(I). The crystal of compound 2 is of monoclinic system, space group P21/n, with a = 13.050(4), b = 20.577(5), c = 13.323(4)A,β = 113.578(3)°, V = 3227.2(14)A3, Z = 2, C64H48F12Mn2N10O8P2, Mr = 1484.94, Dc = 1.528 g/cm^3, F(000) = 1508.0, Rint= 0.0295, T= 293(2) K,μ = 0.539 mm^-1, the final R = 0.0629 and wR = 0.1789 for 5298 observed reflections with I 〉 2σ(I). Compounds 1 and 2 are linear trinuclear and dinuclear manganese complexes respectively, which are both bridged by carboxylate groups of the ligands.  相似文献   

20.
The compound [Cd(phen)(NCS)(SCN)]n(phen = 1,10-phenanthroline) was synthe- sized under hydrothermal conditions and characterized by IR and single-crystal X-ray diffraction. The complex is of monoclinic, space group C2/c with a = 14.607(3), b = 10.505(2), c = 10.631(2)A,β = 115.14(3)^o, V = 1476.8(5)A^3, C14H8CdN4S2, Mr = 408.76, Z = 4, F(000) = 800, μ = 1.757 mm^-1 and Dc = 1.839 g/cm^3. The final R = 0.0409 and wR = 0.0811 for 1367 observed reflections (I 〉 2σ(I)). In the title compound, each cadmium atom is six-coordinated and connected with two adjacent metal ions by two NCS bridges, creating a zigzag chain. The neighboring chains are linked to each other by the weak van der Waals' S…S interactions and π…π interactions to form a new three-dimensional supramolecular framework.  相似文献   

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