The single crystal of bi（8-hydroxyquinoline） bihydrated cobalt（Ⅱ） complex, [Co（Q）2（H2O）2] （Q=8-hydroxyquinoline ion）, has been synthesized by general method and structurally characterized by single crystal X-ray diffraction. Crystal data: C 18 H 16 CoN2O4, monoclinic, C2/c, a=1.3362（4） nm, b= 0.9412（3） nm, c=1.3543（4） nm, β=109.672（4）°, Z=4. In the complex, Co（Ⅱ） ion is six-coordinated, forming a distorted octahedron. H-bonding and π-π stacking interaction play a significant role to form and stabilize the three-dimensional structure.
A novel flower-like hydrated magnesium carbonate hydroxide,Mg_5(CO_3)_4(OH)_2·4H_2O,with micro-structure composed of individual thin nano-sheets was synthesized using a facile solution route without the use of template or organic surfactant.Reaction time has an important effect on the final morphology of the product.The micro-structure and morphology of Mg_5(CO_3)_4(OH)_2·4H_2O were characterized by means of X-ray diffractometry(XRD),field-emission scanning electron microscopy(FE-SEM).Brunauer-Emmett-Teller(BET)surface areas of the samples were also measured.The probable formation mechanism of flower-like micro-structure was discussed.It was found that Mg_5(CO_3)_4(OH)_2·4H_2O with flower-like micro-structure was a novel and efficient catalyst for the synthesis of diphenyl carbonate(DPC)by transesterification of dimethyl carbonate(DMC)with phenol.
WANG QiangWANG Ke-liWU Xing-longLUO Sheng-junHU Chang-wen
A new three-dimensional supramolecule composed of copper-Schiff base complex, [Cu(naphdien)]Cl·H2O, where naphdien is Schiff base of 2-hydroxy-1-naphthaldehyde and diethyle- netriamine, has been synthesized and determined by single-crystal X-ray diffraction. It belongs to the monoclinic system, space group P21/c, with a = 7.3490(15), b = 7.0847(16), c = 30.845(3), β = 95.33(3)°, V = 1599.0(5)3, Z = 4, C15 H20ClCuN3O2, Mr = 373.33, Dc = 1.551 g/cm3, μ = 1.543 mm-1, F(000) = 772, R = 0.0536 and wR = 0.0927 for 2788 unique reflections with 1659 observed ones (I >2σ(I)). In the crystal structure, mononuclear units [Cu(naphdien)]Cl·H2O are linked into a two-dimensional framework via strong hydrogen bonds, and extended into a three-dimensional supramolecular structure through π-π stacking interactions.
Polyhedron lead hydroxide carbonate(2PbCO3·Pb(OH)2) microcrystals have been prepared in solution phase via a facile method in the presence of surfactant cetyltrimethylammonium bromide(CTAB).All the samples were characterized by powder X-ray diffraction pattern(XRD),field-emission scanning electron microscopy(FE-SEM),high-resolution transmission electron microscopy(HRTEM),and selected area electron diffraction(SAED).The possible growth mechanism was discussed.2PbCO3·Pb(OH)2 microcrystals were found to be a novel and efficient catalyst for the synthesis of diphenyl carbonate(DPC) by transesterification of dimethyl carbonate(DMC) with phenol.Compared with some other catalysts,such as AlCl3,ZnCl2,and Mg5(CO3)4(OH)2,2PbCO3·Pb(OH)2 microcrystals are stable and show relatively high activity at low catalyst amount.When the reaction was carried out at 180 ℃,with a molar ratio of phenol to DMC of 2:1,a reaction time 14 h,and a catalyst amount 0.2%(molar ratio to phenol),the selectivity of DPC and methyl phenyl carbonate(MPC) was 14.7% and 78.8%,respectively.
Two new coordination polymers, [M（phen）（e,a-cis-1,4-chdc）（H2O）]n （M=Mn （1）; M=Cu （2）; chdc=cyclohexanedicarboxylic acid; phen=1,10-phenanthroline）, were prepared under hydrothermal conditions and characterized by IR spectra and single crystal X-ray diffraction analysis. X-ray crystal structural analyses reveal that polymer 1 and 2 are isomorphic and belong to the monoclinic system. C 20H 20MnN2O5, P2（1）/c, a=1.023?5（2） nm, b=0.891?34（19） nm, c=2.046?6（4） mm, β=99.820（3）°, Z=4 for 1; and C 20H 20CuN2O5, P2（1）/c, a=1.000?2（3） nm, b=0.894?9（2） nm, c= 2.027?0（5） nm, β=99.694（3）°, Z=4 for 2. In the structures of 1 and 2, the 1,4-chdc ligand only possesses e,a-cis conformation although there are both cis- and trans-conformations in the raw material.
β-Co(OH)2 and Mg(OH)2 nanoplates were synthesized via a facile template-free hydrothermal approach.The different conditions of preparation and catalytic properties of the products were studied and discussed.The products were characterized by X-ray diffraction,transmission electron microscopy,scanning electron microscopy,selected area electron diffraction(SAED),and gas chromatograph.
SUN Ling-naWANG Ke-liLUO Sheng-junGUO Qing-rongHU Chang-wen
