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1.
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   

2.
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   

3.
Hydrothermal reactions of three aromatic polycarboxylic acids and the transitional metal cations in the presence of phen and 1,4-bib afford three new coordination polymers: [Cd2(bpp)1.5(Hbpp)(phen)2]n (1), [Mn3(Htptc)2(phen)2(H2O)2]n (2), and {[Cu(btc)0.5(1,4- bib)]·2H2O}n(3) (H2bpp = 2,6-bis(4'-carboxyphenyl)-4-phenylpyridine, H4tptc = terphenyl-2,5,2',5'-tetracar- boxylic acid, H4btc =biphenyl-2,2',4,4'-tetracarboxylic acid, phen =1,10-phenanthroline, and 1,4-bib = 1,4-bis(1H-imidazol-1-yl)benzene). Their structures have been determined by single- crystal X-ray diffraction analyses, elemental analyses, IR spectra, and powder X-ray diffraction (PXRD) analyses. In compound 1, the CdII cations are linked by bpp2- to form one ladder structure, based on which a 3D network is constructed with the help of non-covalent interactions. The topology of 2 is a 3D (3,4,5)-connected framework with the Point Schl?fli symbol of (42.6)2(43.62.8)(45.64.8)2. Compound 3 shows an unprecedented 3D (4,4)-connected framework with the Point Schl?fli symbol of (64.82)2(65.8). Moreover, the luminescent property of 1 has been investigated.  相似文献   

4.
The title compound [Mn(O2CMe)2(phen)2] (phen = 1,10-phenanthroline) 1 has been synthesized and structurally determined by single-crystal X-ray diffraction. The crystal is of orthor- hombic, space group Pbcn, with a = 12.554(4), b = 10.168(3), c = 17.704(5)A, V= 2259.7(12)A^3 Z = 4, C28H22MnN4O4, Mr= 533.44, Dc= 1.568 g]cm^3, F(000) = 1100, Rint = 0.0242, T= 293(2) K and p = 0.631 mm^-1. The final R = 0.0687 and wR = 0.1960 for 2046 observed reflections with I 〉 20(/). The structure of the complex consists of one Mn(II) core coordinated by two bidentate-bound CH3COO^- groups and two η^2-phen groups forming an eight-coordinate geometrical configuration.  相似文献   

5.
Compounds [Zn(2,2'-bipy)(L)Cl]2 1 and [Zn(phen)(L2)]2 2 (2,2'-bipy = 2,2'-bipyridine, HL = 3-methylbenzoic acid, phen = 1,10-phenanthroline) have been synthesized under hydrothermal conditions. 1: monoclinic, space group C2/c, a = 20.240(4), b = 9.2960(19), c = 17.904(4)A, β = 92.63(3)°, V = 3365.1(12) A^3, C36H30Cl2N4O4Zn2, Mr = 784.32, Z = 4, Dc = 1.548 g/cm^3, μ = 1.631 mm^-1, F(000) = 1600, the final R = 0.0367 and wR = 0.1289 for 3867 observed reflections (I 〉 2σ(I)). 2: monoclinic, space group C2/c, a = 23.035(5), b = 9.0395(18), c = 23.799(5) A, β = 98.55(3)°, V = 4900.6(17)A^3, C56H44N4O8Zn2, Mr = 1031.73, Z = 4, Dc = 1.398 g/cm^3, μ = 1.039 mm^-1, F(000) = 2128, the final R = 0.0540 and wR = 0.1287 for 5002 observed reflections (I 〉 2σ(I)). The two compounds have the same space group and similar isolated dinuclear structure, but different space packing structures are formed by different weak intermolecular interactions. Mo- reover, IR and luminescence spectra are also employed to study the crystal structures and pro- perties of these two compounds.  相似文献   

6.
温德才  谢静  姜秀榕 《结构化学》2009,28(3):279-282
A new coordination polymer [Mn{5-(NO2)sal}2(phen)]n (5-(NO2)sal = 5-nitrosalicylate, phen = 1,10-phenanthroline) was synthesized by a hydrothermal reaction and characterized by elemental analysis, IR and X-ray single-crystal diffraction. The title complex crystallizes in orthorhombic, space group Pbcn with α = 25.747(8), b = 13.220(4), c = 7.009(3) A, V= 2386(1)A^3, Z = 4, R = 0.0427 and wR = 0.0890. The 5-nitrosalicylate anions doubly bridge the Mn(Ⅱ) atoms to form a one-dimensional polymeric chain with repeated eight-membered ring units (Mn-O-C-O)2. The crystal structure is stabilized by intra- and interchain hydrogen bonding interactions. The cyclic voltammetric behavior of the title complex is also reported.  相似文献   

7.
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   

8.
A new hybrid polyoxometalate-based complex, [Cu^I(phen)214(SiW12O40) (phen = 1,10-phenanthroline), has been synthesized by hydrothermal method and characterized with the aid of elemental analysis, IR, UV spectra and thermal analysis studies. The result of X-ray crystallography analysis exhibits that the title compound crystallizes in the orthorhombic space group P212121, and the formula is C96H64N16Cu4SiW12O40. Crystal data: a = 18.3574(14), b = 21.1952(16), c = 27.992(2)A, Mr = 4570.08, V = 10891.4(14)A^3, Z = 4, Dc = 2.787 g/cm^3,μ = 13.478 mm^-1, R = 0.0364, wR = 0.0638 (I 〉 2σ(I)) and F(000) = 8360. The complex consists of one α-Keggin anion [SIW12O40]^4- and four discrete [Cu^I(phen)2]^+ cations. The valence sum calculations for the Cu atoms suggest that all four Cu atoms are in the +1 oxidation state.  相似文献   

9.
A novel Mn(Ⅱ) complex Mn2(phen)2(p-MBA)4(H2O) has been hydrothermally synthesized by the reaction of p-methyl benzoic acid (p-MBA) with 1,10-phenanthroline (phen). Crystal data for this complex: monoclinic, space group C2/c, a= 2.3328(3), b =1.5549(2), c = 1.5557(2) nm, β = 121.726(2)°, V= 4.7997(11) nm^3, Mr = 1028.85, Dc = 1.424 g/cm^3, Z = 4, F(000) = 2128, μ(MoKa) = 0.590mm^-1, GOOF = 1.060, R = 0.0333 and wR = 0.0767. In the crystal, each Mn(Ⅱ) ion is coordinated by two nitrogen atoms from one o-phenanthroline molecule, three oxygen atoms from three p-methyl benzoic acids and one oxygen atom from one water molecule, giving a six-coordinate distorted octahedral coordination geometry. Two neighboring Mn(Ⅱ) ions are bridged by two p-methyl benzoic acid groups and one water molecule, and their end positions are respectively coordinated by one 1,10-phenanthroline and one p-methyl benzoic acid molecule, giving a binuclear cage structure, of which the Mn(Ⅱ)…Mn(Ⅱ) distance is 0.3502 nm.  相似文献   

10.
A new complex [Cu(phen)3][(C6H4)2C(OH)COO]2·6H2O was prepared by selfassembly 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)°, V = 2.8914(7) nm^3, Dc = 1.340 g/cm^3, 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   

11.
李秀梅  王志涛  刘博  王庆伟  周实 《结构化学》2009,(10):1257-1260
A metal-organic coordination compound formulated as [Zn(pzdc)(phen)]n·nH2O 1 (H2pzdc = pyrazine-2,3-dicarboxylic acid, phen = 1,10-phenanthroline) has been hydrothermally synthesized and structurally characterized by elemental analysis, IR, fluorescence spectrum and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group P21/n with a = 11.607(2), b = 11.719(2), c = 13.140(3)A^°, β = 110.707(3)°, V= 1671.9(6)A^°3, C18H12ZnN4O5, Mr= 429.69, De = 1.707 g/cm^3,μ(MoKa) = 1.511 mm^-1, F(000) = 872, Z = 4, the final R = 0.0356 and wR = 0.0853 for 2713 observed reflections (I 〉 2σ(I)). It exhibits an interesting two-dimensional layer structure and shows yellow photoluminescent property at room temperature.  相似文献   

12.
Two new mixed-ligated metal phosphonates, M2(pbtcH)(phen)2(H2O)2 [M(Ⅱ)=Co (1), Ni (2)] (pbtcH5 = 5-phosphonatophenyl-1,2,4-tricarboxylic acid, phen = 1,10-phenanthroline), have been syn- thesized and characterized. Both show one-dimensional double chain structures, where the M(phen)(H2O) moieties are chelated and bridged by pbtcH4 through the carboxylate and phosphonate oxygen atoms. The chains are connected by hydrogen bonding interactions and π-π stacking, forming a three-dimensional supramolecular structure. The IR and magnetic properties of the two compounds are also investigated.  相似文献   

13.
Two coordination polymers, namely {[Co(L)(H2O)]·H2O}n (1) and [Mn(L)(phen)]n (2, H2L = 5-(pyridin-4-yl)isophthalic acid, phen = 1,10-phenanthroline), have been hydrothermally synthesized and characterized by elemental analysis, IR, TG, magnetic properties, and single-crystal X-ray diffraction. 1 belongs to the triclinic system, space group Pī with α = 7.2188(7), b = 10.0835(8), c = 10.2069(7) ?, α = 113.713(7), β = 99.490(7), γ = 104.516(8)o, V = 628.24(9) ?3, C13H11NCoO6, Mr = 336.16, Z = 2, Dc = 1.777 Mg/m3, μ(MoKα) = 1.395 mm–1, F(000) = 342, S = 1.041, the final R = 0.0381 and wR = 0.0819 for 3744 observed reflections (I 〉 2σ(I)) and R = 0.0448 and wR = 0.0874 for all data. 2 belongs to the monoclinic system, space group P2/c with α = 12.9185(3), b = 10.4343(2), c = 31.7650(6) ?, β = 101.282(2)o, V = 4199.08(13) ?3, C50H30N6Mn2O8, Mr = 952.68, Z = 4, Dc = 1.507 Mg/m3, μ(MoKα) = 5.447 mm–1, F(000) = 1944, S = 1.128, the final R = 0.1003 and wR = 0.1052 for 8247 observed reflections (I 〉 2σ(I)) and R = 0.2595 and wR = 0.2625 for all data. Single-crystal X-ray diffraction studies show that compound 1 features a 2D sheet structure based on a dicobalt(II) subunit, which is further extended into a 3D metal-organic supramolecular framework by O–H… hydrogen bond. Compound 2 also possesses a 2D sheet, which is held together into a 3D supramolecular architecture via C–H… hydrogen bond and π-π stacking interactions. Magnetic studies for compound 2 show antiferromagnetic coupling between the adjacent metal centers, with J = –11.8 cm–1 and g = 2.12 for 2.  相似文献   

14.
Two lead(ll) compounds, [Pb(qlc)(phen)2(NO3)]e-H20 (1) and [Pb(qlc)z(phen)]-3H20 (2) (Hqlc = quinoline-3-carboxylic acid, phen = 1,10-phenanthroline), were synthesized and charac- terized by elemental analysis, single-crystal X-ray diffraction, IR and thermogravimetric analysis. Crystal 1 is of monoclinic, space group C2/c with a = 25.246(5), b = 12.543(3), c = 18.917(4) A, β = 105.77(3)°, V= 5765(2) A3, Z = 4, C68H46N12OllPb2, Mr = 1621.53, Dc = 1.886 g.cm-3,/.t(MoKa) = 5.912 mm-1, F(000) = 3152, GOOF = 1.080, the final R = 0.022 and wR = 0.0571 for 4822 observed reflections (1 〉 2a(/)). Crystal 2 is oftriclinic, space group Pi with a = 8.7883(10), b = 11.7031 (13), c = 15.9320(17) A, a = 69.9400(10), fl = 78.9780(10), 7 = 79.1650(10)°, V = 1497.4(3) A3, Z = 2, C32H26NaO7Pb, Mr. = 785.71, Dc = 1.729 g.cm-s, p(MoKa) = 5.688 mm-1, F(000) = 756, GOOF = 1.106, the final R = 0.0313 and wR = 0.088 for 59i5 observed reflections (1 〉 2σ(I)). Single-crystal X-ray diffraction analysis reveals that 1 exhibits a two-dimensional (2D) layer based on π-π stacking interactions between phen. Simultaneously, the adjacent 2D layers are assembled via π-π stacking interactions between phen and quinoline tings into a 3D supramolecular structure. The zero- dimensional structure of 2 is also further extended by π-π interactions to form a 2D supramolecular layer. Furthermore, these two compounds exhibit photoluminescence at room temperature in the solid state and their photocatalytic activities have been studied by degradation methylene blue.  相似文献   

15.
[Co^11(phen)3]2[{(ZnW12O40)Co^11(phen)2(H2O)}2Co^11(trien)2(NaH2O)2]·3H2O was synthesized via hydrothermal technique and characterized with elemental analyses, IR spectroscopy, TGA-DTA, and variable temperature magnetic susceptibility. The compound crystallized in the monoclinic system with the space group P21/n, a=1.8210 nm, b=2.3592 nm, c=2.2932 nm, β=110.31°, V=9.239 nm^3, Z=2, R1=0.0827. The compound consists of two coordination cations, three lattice water molecules, and a macroanion [{(ZnW12O40)Co(phen)2(H2O)}2Co(C6H18N4)2·(NaH2O)2]^4- in which each supported Keggin anion [(ZnW12O40Co^11(phen)2(H2O)]^4- acts as a ligand to coordinate to central bridging Co^2+ ion via a terminal oxygen atom. Hydrogen bonds are responsible for the construction of 3D architecture of the compound. The compound is paramagnetic with a weak antiferromagnetic interaction(0=-46.796 K).  相似文献   

16.
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   

17.
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   

18.
A new metal-organic coordination polymer [Cd(5-hip)(phen)]n·nH2O 1 has been hydro- ermally synthesized and characterized by elemental analysis, IR, TG and single-crystal X-ray diffraction. The crystal of the complex crystallizes in monoclinic, space group P2/n with a = 8.8071(17), b =12.386(2), c = 16.981(3) A, β = 100.182(2)°, V = 1823.2(6) A^3, Mr=. 490.73, Dc =1.788 g/cm^3,μ(MoKa) = 1.240 mm^-1, F(000) = 976, Z= 4, the final R = 0.0458 and wR = 0.1373 for 2864 observed reflections (I 〉 2σ(I)). The Cd atoms are coordinated by two N atoms from the phen ligands and four O atoms from 5-hydroxyisophthalate ligands in a highly distorted octahedral geometry.  相似文献   

19.
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   

20.
本文通过溶剂热方法合成了四个新的混合配体配合物[Zn(dba)(bpy)]n(1),{[Zn(dba)(phen)]·2H20}。(2),[Cd(dba)(bpy)(H20)2](3)和[Cd2(dba)2(phen)2]n(4)(H2dba=2,5-二羟基对苯二乙酸,bpy=2,2'-联吡啶,phen=1,10。菲咯啉).对这四个化合物进行了单晶衍射、红外光谱、元素分析和粉末X-射线衍射等表征.化合物1和2具有1D无限链状结构,化合物3为单核构型,化合物4是由H2dba配体桥联的双核对称单元组装成的2D网络结构.对这几个化合物的荧光性质进行了研究.  相似文献   

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