The hydrothermal reaction of 1,2-dicyanobenzene with NaN3 in the presence of CuC12, 2,2'-bipyridine and H2O affords a novel dinuclear copper(Ⅱ)-ditetrazolate, [Cu(bpy)- (pdtz)]2 (Hpdtz = 5,5"-1,2-phenylene-ditetrazole, bpy = 2,2'-bipyridine). The pdtz ligand is generated in situ through Sharpless 2+3 cycloaddition reaction. Its crystal structure was determined by single-crystal X-ray diffraction method. The crystal crystallizes in the monoclinic system, space group P211n with a = 8.2096(16), b = 18.580(4), c = 11.838(2) A, β = 103.12(3)°, V = 1758.5(6) A^3, Z = 2, Mr = 863.83, Dc = 1.631 g/cm^3, F(000) = 876 and μ = 1.272 mm^-1. In this novel dinuclear structure, the pdtz ligand adopts a peculiar μ2-η1,η2 coordination mode.
HUANG Xi-He SHENG Tian-Lu XIANG Sheng-Chang FU Rui-Biao HU Sheng-Min LI Ya-Min WU Xin-Tao
Hydrothermal reaction of 1,2,4-benzenetricarboxylic acid, and MnCl24H2O with 1,10-phenanthroline gave the title complex, [Mn(phen)(m-phth)]n, which crystallizes in the monoclinic system, space group P2/c with a=0.83582(3) nm, b=1.04246(4) nm, c=1.87777(7) nm, =100.314(2), V=1.60968(10) nm3, Z=4, and the final R=0.0576, wR=0.1294. In the complex, each Mn(II) ion is coordinated to four O atoms of carboxylate groups and two N atoms of phen. Isophthalate was generated in situ through the loss of one carboxylate group of 1,2,4-benzenetricarboxylic acid under the hydrothermal condition. Each isophthalate is bound to three manganese atoms through O atoms of carboxylate in bridging and chelating fashion, affording manganese(II) pairs that are linked by the isophthalate group to yield a zig-zag chain along the c-axis.
A novel copper molybdate with mixed ligands, [{(Cu·phen)e(tp)} {(Cu·phen·H2O)2(tp)} {Mo4O14}(phen = 1,10-phcnanthroline, tp = tercphthalate) 1, has been hydrothermally synthesized and structurally characterized. The crystal belongs to monoclinic system, space group P2l/c with a = 13.1711(7), b = 19.6132(10), c= 13.6910(7) A, β = 117.6870(10)°, V= 3131.8(3) A^3, Z= 2, C64H44Cu4MoaN8O24, Mr= 1946.99, D, = 2.065 g/cm^3, F(000) = 1920,μ(MoKa) = 2.198 mm ^1, R = 0.0810 and wR = 0.2012 for 4233 observed reflections (I 〉 2σ(I)). The structural analysis indicates that the title compound contains a discrete tetramolybdate cluster decorated with copper colnplcx fragments and tp ligands bridging the clusters into a wave-like layer. The hydrogen bonding between adjacent layers further extends the COlnpound into a 3-D framework.
A novel Cu(II)-2,2'-bipy-supported (bipy = bipyridine) mixed valence decatungstate, [Cu(2,2'-bipy)2]2Na2W6^VW4^VIO30·2H2O 1, has been synthesized and structurally characterized by X-ray analysis. The crystal of 1 is of triclinic, space group P1^- with a= 10.9393(10), b = 12.0492(2), c = 12.3783(2)A, a = 80.631(10), β= 70.226(10), γ= 72.329(9)^o, V = 1459.64(4)A^3, Z = 1, Dc = 3.582 g/cm^3, F(000) = 1404, R = 0.0553 and wR = 0.1242 for 4607 observed reflections (I 〉 2σ(I)). The EPR spectrum of 1 indicates that its unpaired electrons are placed in the dx2-y2 orbital of the ground state of Cun. Furthermore, compound 1 shows an antiferromagnetic interaction.
POMs,as building blocks to construct the solid-state materials with versatile organic ligands or charge compen...
Yi-Ming Xie Can-Zhong Lu~* The State Key Laboratory of Structural Chemistry,Fujian Institute of Research on the Structure of Matter,Chinese Academy of Sciences,Fuzhou 350002,China.
Coordination polymers with different networks,which have potential functions, including nonlinear optics,catal...
Zhen-Lan Fang Qi-Sheng Zhang Xiao-Yuan Wu Shan-Ci Chen Can-Zhong Lu~* The State Key Laboratory of Structure Chemistry,Fujian Institute of Research on the Structure of Matter,The Chinese Academy of Science,Fuzhou,Fujian,350002,Pepole's Republic of China
A new compound, (H3O)3{Na3(H2O)13(Cu(Gly)2)2(H2W12O42)}·11H2O (1), has been synthesized and structurally characterized, which represents the first example of a polyoxotungstate-surface being decorated with amino acid ligand. Two cis-{Cu(Gly)2}2+ engraft into the (H2W12O42)10- with Cu-O bond of 0.241 2(7) nm, and Na+ ions linked these (Cu(Gly)2)2(H2W12O42)6- clusters into a one-dimensional chain. CCDC: 278000.
The hydrothermal reaction of 1,2-dicyanobenzene with NaN3 in the presence of Cd(NO3)2 affords a novel 2D cadmium tetrazolyl-benzoate, {Cd(tzbz)(H2O)}n (H2tzbz is 2-(5-tetrazolyl)-benzoate). The tzbz ligand is generated in situ through the [2+3] Sharpless cycloaddition reaction and hydrolyzation. Its crystal structure was determined by single-crystal X-ray diffraction method. The crystal crystallizes in the orthorhombic system, space group Pbca with a = 9.6659(19), b = 7.6366(15), c = 25.964(5)A, V= 1916.5(7)A^3, Z= 8, Mr = 318.57, Dc = 2.208 g/cm^3, F(000) = 1232 and p = 2.276 mm^-1. The Cd(Ⅱ) atom is coordinated by four tzbz ligands and one water molecule to form a severely distorted pentangle bipyramid. While each tzbz ligand connects to four Cd(Ⅱ) atoms in a μ4-η1, η, η1, η1, η1 coordination mode to construct a 2D architecture of the title complex. Additionally, the title complex exhibits strong fluorescence at room temperature in the solid state.
HUANG Xi-He SHENG Tian-Lu XIANG Sheng-Chang FU Rui-Biao HU Sheng-Min LI Ya-Min WU Xin-Tao
Crystal engineering of metal complexes,especially coordination polymers has been greatly developed in the past...
Shan-Ci Chen Xiao-Yuan Wu Zhen-Guo Zhao Can-Zhong Lu~* The State Key Laboratory of Structural Chemistry,Fujian Institute of Research on the Structure of Matter,Chinese Academy of Sciences,Fuzhou 350002,China.