The title compounds Mo3S4(dtp)3(o-CH3OC6H4COO)(Py) 1 and Mo3S(dtp)3(p-HOC6H4COO)(DMF)稥tOH 2 (dtp = diethyldithiophosphate) were synthesized by thereactions of Mo3S4(dtp)4(CH3CN) and Mo3S4(dtp)3(CH2ClCOO)(Py) with o-methoxylbenzoic acid and p-hydroxybenzoic acid, respectively. Their crystal structures were determined by X-ray diffraction analysis. The crystal data for compound 1: Mo3S10P3C25H42O9N, monoclinic P21/n, Mr = 1201.93, Z = 4, a = 14.164(1), b = 23.065(2), c = 14.732(1) ? = 109.677(1) ? V = 4532(1) ?, D= 1.762 gcm-3, = 1.428 mm-1, F (000) = 2408, R = 0.0739, wR = 0.1528 for 3552 observed reflections (I > 2); and for compound 2: Mo3S10P3C24H48O11N, triclinic P ? Mr = 1227.96, Z = 2, = 10.2098(3), b = 14.3333(4), c = 18.1711(5) ? = 94.694(1), = 102.166(1), = 110.665(1) , V = 2396.5(1)3, Dc = 1.638 gcm-3, = 1.350mm-1, F (000) = 1184, R = 0.0445, wR = 0.1281 for 6597 observed reflections (I > 2). Intermolecular S…S interactions are observed between the molecules of compound 1 while intramolecular O…HC and intermolecular S…HC hydrogen bondings are found in the crystal packing diagram of compound 2.
A novel 2-D sheet inorganic-organic hybrid cadmium polymer,[CdBr2(bpdo)]n (bpdo=N,N'-O,O-4,4'-bipyridine) has been hydrothermally synthesized and characterized by elemental analysis,IR and single-crystal X-ray diffraction. The crystal crystallizes in monoclinic,space group C2/c,with a=16.336(3),b=3.9904(5),c=18.479(3),β=91.640(6)°,Mr= 460.40,V=1204.1(3)3,Z=4,Dc=2.540 g/cm3,μ=8.439 mm-1,F(000)=864,R=0.0314 and wR=0.0733 for 1069 observed reflections (I > 2σ(I)). X-ray diffraction reveals that the title compound consists of the 2-D inorganic-organic hybrid sheet constructed from [CdBr2]n chains and bpdo bridges in the packing motif of…ABAB….The title compound exhibits intense blue photoluminescence in the solid state at room temperature.
The title compound (C6H5NH2)2PdCl2 was prepared by the reaction of N-phenylbenzaldimine with dichlorobis(benzonitrile) palladium (Ⅱ) in methanol and its structure was characterized by single-crystal X-ray diffraction. The title complex crystallizes in monoclinic system, space group P21/c, C12H14Cl2N2Pd, Mr = 363.55, a = 6.0668(7), b = 4.7691(5), c = 23.006(3) ? b = 95.118(2)? V = 662.99(13) ?, Z = 2, Dc = 1.821 g/cm3, m = 1.780 mm-1, F(000) = 360, the final R = 0.0624 and wR = 0.1271 for 850 observed reflections. Two bifurcated intermolecular NH…Cl hydrogen bonds are observed, forming a strip structure.
Two new copper coordination polymers [Cu(μ2-4,4?-bipyridine)(NO2)2]n (C10H8- N4O4Cu, Mr = 311.75) 1 and [Cu(μ2-4,4?-bipyridine)2(H2O)2]n?2n(4,4?-bipyridine)?2nClO4?nH2O (C40H38N8O11Cl2Cu, Mr = 941.22) 2 were synthesized by hydrothermal reaction and determined by X-ray diffraction method. Compound 1 crystallizes in monoclinic, space group P2/m with a = 4.7740(10), b = 11.039(2), c = 5.6752(14) ?, β = 91.394(9)o, V = 299.00(11) ?3, Z = 1, Dc = 1.731 g/cm3, F(000) = 157 and μ(MoKa) = 0.7107 mm-1. Compound 2 crystallizes in monoclinic, space group P2/n with a = 12.916(2), b = 11.149(1), c = 15.006(2) ?, β =106.642(6)o, V = 2070.3(5) ?3, Z = 2, Dc = 1.510 g/cm3, F(000) = 970 and μ(MoKa) = 0.7107 mm-1. In the structure of compound 1, the metal atom is in a slightly distorted octahedral CuO4N2 geometry surrounded by four O atoms of two NO2 ligands in the equatorial positions and two N atoms from 4,4?-bipyridine ligands in the axial sites, and the 4,4?-bipyridine ligands bridge the neighboring Cu2+ atoms to form polymeric chains in the lattice. Compound 2 has a 2D square-grid network structure. The square grids are superposed on each other to form a channel framework. The square cavity has dimensions of 11.148(2)? ×11.229(3)?. Every two guest 4,4?-bipyridine molecules are clathra- ted in each hydrophobic host cavity and further stabilized by π-π stacking and hydrogen bonding interactions.
The title compound, [Cu(phen)2(SO4)(H2O)]·0.5C4H4O4·7H2O (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 P1 with a = 11.4827(2), b = 11.9086(2), c = 13.77350(10) ?, α = 80.6830(10), β = 66.6480(10), γ = 64.0480(10)o, V = 1554.63(4) ?3, Mr = 722.17, Z = 2, Dc = 1.543 g/cm3, μ = 0.845 mm-1, F(000) = 750, R = 0.0349 and wR = 0.0837 for 4754 observed reflections (I > 2σ(I)). The compound contains a six-coordinated copper(II) center, which is surround by four N atoms of two phen ligands (Cu–N distances in the range of 1.997(2)～2.225(2) ), one sulfate O atom (Cu–O = 2.0037(17) ) and one water O atom (Cu–O(5w) = 2.719(2) ?) in a distorted octahedral geometry. Extensive hydrogen-bonding interactions are involved in water molecules, ligated sulfate anions and fumaric acid molecules. In addition, π-π 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.
The title compound, [Zn(AIP)(4,4-bipy)0.5(H2O)]n·0.75nH2O 1, was synthesized via the hydrothermal reaction of Zn(OAc)2 with 5-aminoisophthalic acid (H2AIP) and characterized by elemental analysis and infrared spectra. The complex crystallizes in monoclinic system, space group P21/c with a = 12.672(1), b = 7.6557(4), c = 16.181(1) , β = 109.187(2)o, V = 1482.6(2) 3, Z = 1, C52H52N8O23Zn4, Mr = 1418.58, Dc = 1.589 g/cm3, F(000) = 724 and μ(MoKα) = 1.685mm-1. The final R = 0.0702 and wR = 0.1524 for 1847 observed reflections with I > 2σ(I), and R = 0.0873 and wR = 0.1664 for all data. X-ray diffraction studies reveal that the title compound has an interesting 2D microporous architecture with guest water molecules inside the channel.
A new zinc polymer, {Zn(O2CC12H8CO2)(H2O)}n or {Zn(DPHA)(H2O)}n (O2CC12- H8CO2, DPHA = 1,1?-biphenyl-2,2?-dicarboxylate dianion) has been synthesized under hydrother- mal conditions. The crystal is of monoclinic, space group P21/c with a = 12.8418(5), b = 5.9505(2), c = 17.2989(5) ?, β = 104.020(2)o, V = 1282.52(8) ?3, C14H10O5Zn, Mr = 323.61, Z = 4, Dc = 1.676 g/cm3, μ = 1.930 mm-1, F(000) = 656, R = 0.0766 and wR = 0.1871 for 1775 observed reflections (I > 2σ(I)). It consists of Zn2(DPHA)2(H2O)2 units, which are further extended into a one-dimensional double helical-chain polymer via Zn–O bonding. The hydrogen bonding interactions extend the helical chains into a two-dimensional layer structure.
YIN Pei-Xiu ZHANG Jian WEN Yi-Hang CHENG Jian-Kai LI Zhao-Ji YAO Yuan-Gen
A novel 2-D lead-containing hybrid compound, [(PbCl2)(μ-Pyz)1/2]n (Pyz = py- razine) 1, has been synthesized by the hydrothermal assembly of pyrazine with lead chloride. Elemental analysis and X-ray crystal structure analyses were carried out for the structural deter- mination and characterization of the title compound. Compound 1 crystallizes in orthorhombic, space group Ibam, with a = 19.5558(18), b = 7.1939(6), c = 7.5449(6) , V = 1061.44(16) 3, C2H2Cl2NPb, Mr = 318.14, Z = 8, Dc = 3.982 g/cm3, μ = 32.63 mm-1, F(000) = 1096.0, R = 0.0368 and wR = 0.0901 for 623 observed reflections (I > 2σ(I)).
