A new Ni（Ⅱ） complex [Ni2（salen）2]·（NCS）·NH4 （salen = N,N＇-bis（salicylideneamino）ethanato） has been prepared and structurally characterized by elemental analysis, IR spectra and single crystal X-ray diffraction. It crystallizes in the orthorhombic system, space group Pbca with a = 16.8725（13）, b = 19.0046（15）, c = 20.0583（16）A, Z = 8, V = 6431.8（9）A^3, C33H32N6Ni2O4S1, Mr = 726.13, Dc = 1.500 g/cm^3, F（000） = 3008, μ = 1.284 mm^-1, the final R = 0.0394 and wR = 0.0767 for 4449 observed reflections with I 〉 2σ（I）. The complex involves a N,N＇-ethylene-bis（salicylaldiminato） Schiff base, an isothiocyanato anion and an ammonium cation. The nickle（II） ion adopts a distorted square coordination geometry with N2O2 set of Schiff base ligand. The complexes are linked into a dimmer via intermolecular hydrogen bonds and the [Ni（salen）] moieties are connected together to form a 2-D layer structure by intermolecular N-H…O hydrogen bonds and π-π stacking. Cyclic-voltammetry method was used to characterize electrochemically the complex.
The crystal structure of [MnCl(NIT-1′-MeBzIm)] (NIT-1′-MeBzIm=2-{2′-[(1′-methyl) benzimidazolyl]}-4,4,5,5-tetr...
WANG Li-ya~(a,b) CHENG Jiang-tao~(a,b) JIANG Kai~b a Department of Chemistry, Luoyang Normal University, Luoyang (471022) China b College of Chemistry and Environmental Science, Henan Normal University, Xinxiang (453002) China
A novel compound, {[Cu2（nbdc）2（4,4＇-bpy）2（H2O）2]·2H2O}n（H2nbdc = 4-nitrobenzene-1,2-dicarboxylic acid, 4,4＇-bpy = 4,4＇-bipyridine）, was hydrothermally synthesized and characterized by elemental analysis, IR spectroscopy, thermogravimetric analysis（TGA）, and single-crystal X-ray diffraction. The complex is of orthorhombic system, space group Pbcn with a = 32.222（7）, b = 7.8503（16）, c = 28.389（6）, V = 7181（3）3, Dc = 1.720 g/cm3, Mr = 929.74, Z = 8, F（000） = 3792, μ = 1.273 mm-1, the final R = 0.0591 and wR = 0.1378 for 4548 observed reflections with I 〉 2σ（I）. The compound exhibits a 3D self-penetrating framework with bcu net topology, in which the（46·48）-networks are joined by the H2nbdc and 4,4＇-bpy linkers.
A novel coordination polymer {[Zn（ts-gln）（bipy）].3H2O}n （ts-glnH2 = N-p-tolysulfonyl-glutamine, bipy = 2,2′-bipyridine） has been prepared and structurally characterized by X-ray diffraction method. It crystallizes in orthorhombic, space group P212121 with a = 8.2622（5）, b =16.6244（10）, c = 18.2807（10） A, V = 2510.9（3） A^3, C22H2N4O8SZn, Mr = 573.91, Z = 4, Dc = 1.518 g/cm^3, μ（MoKα） = 1.115 mm^-1, F（000） = 1192, the final R = 0.0262 and wR = 0.0662 for 5691 independent reflections with Rint = 0.0240. The zinc（Ⅱ） atom is coordinated by N（3） and N（4） atoms of a bipy molecule, two carboxylate O（1） and O（2A） and amino N（ 1 ） atoms of ts-gln ligands, resulting in a square-pyramidal geometry. The title complex consists of an infinite zigzag chain of zinc（Ⅱ） ions linked by the carboxylate of N-p-tolysulfonyl-glutamine.
MA Lu-FangHUO Xian-KuanWANG Li-YaFAN Yao-TingZHANG Su-Yun
Utilizing N-[（4-carboxyphenyl）-sulfonyl]glycine （abbreviated as cbsglyH3）,a new cobalt complex [Co（cbsglyH）（bipy）2]3H2O （bipy = 2,2＇-bipyridine） has been synthesized under mild conditions and characterized by IR,elemental analysis,thermogravimetric analysis and X-ray diffraction analysis. It crystallizes in the monoclinic system,space group C2/c with a = 34.978（3）,b = 12.0437（11）,c = 20.0041（19） ,β = 122.2990（10）°,V = 7123.0（11） 3,Z = 8,C29H28CoN5O9S,Mr = 681.55,μ = 0.593 mm-1,Dc = 1.271 Kg/m3,F（000） = 2816,the final R = 0.0434 and wR = 0.1351. The title complex is a monomeric compound which is further assembled by intermolecular hydrogen bonds into a 3-D supramolecular network. Thermogravimetric analysis illustrates that this complex begins decomposing at 100 ℃ and decompounding completely at 560 ℃.
The compound 2,4,4,9,11,11-hexamethyl-1,5,8,12-tetraazacyclotetradecane-1,8-diene(1) was synthesized by new method with high yield(95.2%),and its complex with Cu(II) and SCN-was also obtained.The structures of both the ligand and the complex were characterized by IR,elemental analysis,and X-ray diffraction.The crystal of the title compound(2) belongs to monoclinic system,space group P21/n,Mr=501.53,a=1.28883(11) nm,b=1.13462(10) nm,c=1.58128(13) nm,β=102.7430(10)°,V=2.2554(3) nm3,Z=4,d=1.477g/ cm3,F(000)=1052.R1=0.0360,wR2=0.0976[I>2σ(Ⅰ)].The copper atom is five–coordinated with four nitrogen atoms from compound 1 and one nitrogen atom from thiocyanate to form a tetragonal pyramid structure.
