The title compound, [Cu(phen)(2)(SO4)(H2O)]center dot 0.5C(4)H(4)O(4)center dot 7H(2)O (phen = 1, 10-phe-nan throline and C4H4O4 = fumaric acid), has been synthesized and characterized by single-crystal X-ray diffraction. The crystal is of triclinic, space group P (1) over bar with a = 11.4827(2), b = 11.9086(2), c = 13.77350(10) angstrom, alpha = 80.6830(10), beta = 66.6480(10), gamma = 64.0480(10)degrees, V = 1554.63(4) angstrom(3) , M-r = 722.17, Z = 2, D-c = 1.543 g/cm(3), mu = 0.845 mm(-1), F(000) = 750, R = 0.0349 and wR = 0.0837 for 4754 observed reflections (1 > 2 sigma(l)). The compound contains a six-coordinated copper(H) center, which is surround by four N atoms of two phen ligands (Cu-N distances in the range of 1.997(2)similar to 2.225(2) angstrom), one sulfate O atom (Cu-O = 2.0037(17) angstrom) and one water O atom (Cu-O(5w) = 2.719(2) angstrom) in a distorted octahedral geometry. Extensive hydrogen-bonding interactions are involved in water molecules, ligated sulfate anions and fumaric acid molecules. In addition, pi-pi interactions via aromatic nitrogen-containing ligands are also discussed. The combination of non-covalent interactions leads to the formation of a 3-D network structure.
Four M-II quinolinato complexes, [Zn-2(quin)(2)(H2O)(3)](n) (1), [Zn(quin)(H2O)(2)](n) (2), [Zn(quin)(H2O)](n), (3) and [Cd(quin)](n) (4) (H(2)quin = 2,3-pyridinedicarboxylic acid or quinolinic acid), have been hydrothermally synthesized and structurally characterized. Xray diffraction analyses reveal that all of these four complexes are constructed from similar rod-like SBUs, [M(quin)](n), (M = Zn or Cd). Complexes I and 2 have similar I-D box-like chains but different packing structures; complex 3 has a 2-D grid-like network and complex 4 has an unusual 2-D bilayer structure. Due to the different structural features, these complexes exhibit different photoluminescent emissions: complex 1 at 439 nm (lambda(ex) = 345 nm),complex 2 at 428 nm (lambda(ex) = 360 nm), complex 3 at 508 nm (lambda(ex) = 304 nm) and complex 4 at 500 nm (lambda(ex) = 324 nm). (c) 2006 Elsevier B.V. All rights reserved.
Three new copper complexes, [CuIICuI(ip)(ipH)(4,4′-bipy)3/2]n (1), [Cu(ip)(4,4′-bipy)]n·3nH2O (2), and [Cu(ipH)2(4,4′-bipy)]n (3), have been hydrothermally synthesized by the reaction of Cu(NO3)2·3H2O with isophthalic acid (ipH2) and 4,4′-bipyridine (4,4′-bipy) under different reaction conditions. Complex 1, a mixed-valence copper(I,II) complex, exhibits a 2-D interpenetrating grid framework, in which five-coordinated CuII and three-coordinated CuI environments are established. The oxidation states of center Cu atoms have been confirmed by X-ray photoelectron spectroscopy (XPS) and electron paramagnetic resonance spectra (EPR). Complex 2 features a 2-D box-like bilayer architecture, in which CuII atoms are linked by ip ligands to form a 1-D double-chain and the resulting chains are further strutted by the 4,4′-bipy ligands. In complex 3, two bridging 4,4′-bipy ligands and two terminal ipH ligands confine the CuII center in a square plane coordination geometry. The whole molecule of 3 was arranged into a 1-D linear chain structure. Additionally, the thermogravimetric analyses (TGA) for complexes 1–3 are also discussed in this paper.
The title compound {Cu-2(pdc)(2)(4,4'-bipy)(H2O)(.)3H(2)O}(2) 1 (H(2)pdc = pyridine-2,6-dicarboxylic acid, also known as dipicolinic acid; 4,4'-bipy = 4,4'-bipyridine) has been synthesized by the hydrothermal reaction and its structure was determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P (1) over bar with a = 7.2278(3), b = 10.6259(4), c = 17.7614(6) Angstrom, a = 79.5990(10), beta = 83.6300(10), gamma = 71.8280(10)degrees, V = 1272.60(8) Angstrom(3), C48H44Cu4N8O24, M-r = 1371.07, Z = 1, D-c = 1.789 g/cm(3), gamma = 1.747 mm(-1), F(000) = 696, R = 0.0397 and wR = 0.1137 for 3938 observed reflections (I > 2sigma(I)). There are two kinds of Cu coordination environments, and each central copper(H) atom is five-coordinated in a distorted square-based pyramidal coordination geometry. Four copper(II) atoms are linked by four pdc and two 4,4'-bipy ligands to form an annular rectangle structure. Extensive hydrogen-bonding interactions involving carboxylate 0 atoms as well as coordinated and free water molecules lead to the formation of a three-dimensional network structure.
A new mixed-valence copper(I,II) coordination complex with [Cu2O8] paddle-wheel dicopper units, [CuIICuI(ip)(ipH)(4,4′- bipy)3/2]n(ipH2=isophthalatic acid; 4,4′-bipy=4,4′-bipyridine) (1), has been hydrothermally synthesized and characterized by single-crystal X-ray diffraction, IR, XPS, EPR and TGA. It exhibits a 2-D interpenetrating grid framework, in which five-coordinated CuII and three-coordinated CuI environments are established.
Two molybdenum cluster compounds, Mo3S4(DTP)(3)(p-chlorobenzoate)(Py)(EtOH)-Et-. (I) (DTP = diethyl dithiophosphate) and Mo3S4 (DTP)(3)(p-chlorobenzoate)(DMF) (II), have been rationally synthesized by the reaction of Mo3S4(DTP)(4)(H2O) or Mo3S4(DTP)(3) (CCl3COO)(Py) with p-chlorobenzoic acid in different solvents. The crystal structures have been determined by X-ray crystallography. The obviously short Mo2-O (of DMF) distance in (II) reveals a stronger covalent bond between Mo3S4 core and the DMF. P-31 NMR studies substantiate that the cluster stability in polar solvents are much improved when mu-DTP or mu-CCl3COO is replaced by p-chlorobenzoate. (C) 2004 Elsevier B.V. All rights reserved.
Two novel Ag(I) complexes, [Ag(PES)(H2O)]n (1) and [Ag(PES)(melamine)] (2), (PES=2-(4-pyridyl)ethanesulfonate), have been synthesized and structurally characterized. Complex 1 shows a novel 2D layer structure and complex 2 shows a zigzag 1D chain via the weak Ag⋯O interactions.
The title compound, [Cu(4,4'-bpy)(H2O)4](C4H2O4)(H2O)4 1, has been synthesized by the reaction of Cu(NO3)2·(3H2O with 4,4'-bipyridine and fumaric acid, and structurally characterized by X-ray diffraction analysis. Its crystal structure belongs to monoclinic, space group C2/c with a = 16.6350(5), b = 11.1667(2), c = 13.1371(4) A, β = 125.144(1)o, C14H26CuN2O12, Mr = 477.91, Z = 4, V = 1995.47(9) A3, Dx = 1.591 g/cm3, μ = 1.160 mm-1, F(000) = 996, R = 0.0331 and wR = 0.0883 for 1765 observed reflections (I > 2σ(I)). A two-dimensional network is formed in complex 1 through the hydrogen bonds and VDW interactions.