A new mononuclear copper (II) complex, [Cu(dbpy)2Cl]OH0.5CH3OH2H2O (dbpy = 4,4?dimethyl-2,2?bipyridine) (C24.50H31ClCuN4O3.50, Mr = 536.52) has been synthesized and its crystal structure was determined by X-ray diffraction method. It crystallizes in monoclinic, space group P2/c with a = 13.383(6), b = 7.653(3), c = 14.164(6) ? b = 105.395(8), V = 1398.7(10) 3, Z = 2, Dc = 1.274 g/cm3, m = 0.908 mm-1, F(000) = 560 and R = 0.0773 for 1467 observed reflections with I>2s(I). Each copper(II) ion is coordinated by two dbpy and one Cl- ion and the coordination geometry can be described as a distorted trigonal bipyramidal arrange- ment.
LI Feng-HuaGAO Dong-ZhaoWU Hong-XingLIN Hua-KuanZHU Shou-Rong
The title compound, 1,2-bis-（p-nitro-phenylsulfonamido）-4,5-dinitrobenzene, was synthesized and characterized by elemental analysis, IR and 1H NMR. A pale yellow prism crystal of C23H26N8O13S2 （Mr = 686.64） was obtained in DMF solution and determined by single-crystal X-ray diffraction method. It crystallizes in triclinic system, space group P1 with a = 10.346（4）, b = 12.210（5）, c = 12.976（5）A , α = 108.220（8）, β = 99.482（4）, γ = 95.490（4）°, V = 1516.7（10） A^3, Z = 2, Dc = 1.504 g/cm^3, F（000） = 712, μ = 0.254, Mr = 686.64, the final R = 0.0561 and wR = 0.1487. One sulfonamido group of the title compound is deprotoned and forms N（3）=C（13）. The crystal involves N,N-dimethylamine from the decomposition of DMF and the proton is transferred to N,N- dimethylamine. It is a strong proof for the characterization of deprotoned recognition compound by X-ray single-crystal structure.
The Cu(II) complex with the ligand 2,9-bis(n-2?5?diazaheptanyl)-1,10-phenan- throline (L) has been synthesized and characterized by single-crystal X-ray diffraction. It crys- tallizes in the monoclinic system, space group P21/n with a = 12.549(4), b = 13.544(4), c = 16.767(5) ? = 107.179(5), C22H32Cl2N6CuO8, Mr = 642.98, V = 2722.5(13) 3, Z = 4, Dc = 1.569 g/cm3, ?= 1.056 mm-1, F(000) =1332, the final R = 0.0733 and wR = 0.1581. The X-ray analysis revealed that the Cu(II) ion is coordinated by six nitrogen atoms of the ligand, in which two nitrogen from phenanthroline and another two from the imine groups near phenanthroline are in the equatorial plane while the two from imine groups at the end of both arms in the axial positions. The coordination geometry can be described as a compressed octahedron.
A new ligand N,N′-bis(2-methelene-1,10-phenanthroline)-3,6-dioxa-1,8-octaneethylenediamine(L) and the corresponding complexes LaL, LaL(Phe), and LaL( Try) were synthesized. The interaction of the complexes with calf thymus DNA was studied by means of electronic absorbance spectra, flurescence spectra, circula r dichroic spectra and viscosity experiments. All the results indicate that the complexes may interact mainly with calf thymus DNA by intercalation and coordina tion binding.
The title compound, 1-（N,N-di-（p-toluenesulfonyl））-amino-2-（N＇-p-toluenesulfonyl）- amino-3,5-dinitrobenzene, was synthesized and structurally determined by single-crystal X-ray diffraction method. It crystallizes in orthorhombic, space group Pna21 with a = 13.723（2）, b = 25.354（4）, c = 8.6565（12） A, V= 3011.9（8） A^3, Z = 4, Mr = 660.68, F（000） = 1368, Dc = 1.457 g/cm^3, μ = 0.309, the final R = 0.0609 and wR = 0.1042. The H atom of N2-H group, which is the unique recognition site to anion, is enveloped by two oxygen atoms and one benzene from two and one p-toluenesulfonyl moieties, respectively.
The title compound, N-（1′-H-pyrrol-2′-ylcarbonyl）-5-amino-1,10-phenanthroline, was synthesized by the reaction of a-pyrrolyl carbonyl chloride and 5-amino-1,10-phenanthroline in pyridine. Determined by X-ray structure analysis, it crystallizes in triclinic system, space group P1 with the following crystallographic data： C20H21N5O3, Mr = 379.42, a = 7.8559（4）, b = 9.1681（6）, c = 14.6818（9） A, α= 73.254（10）,β= 88.938（15）, γ= 68.080（10）°, V= 934.66（10） A3, Z = 2, F（000） = 400, Dc = 1.348 g/cm^3 and p = 0.094 mm-1. The final R = 0.0680 and wR = 0.1419 for 2142 observed reflections with I 〉 2σ（/）, and R = 0.1084 and wR = 0.1643 for all reflections. Two aromatic ring planes （pyrrole and phenanthroline rings） are connected by the amide plane. Two different types of intermolecular hydrogen bonds, O-H…N and N-H…O, exist in the crystal. The title complex molecules are connected through hydrogen bonds and weak π-π stacking interactions to generate a 3-D supramolecule.
