New heteroleptic and homoleptic complexes of the type[Pd（4,5-dmbipy）C12], [Pd（4,5-dmbipy）L2], and [Pd（4,5-dimebipy）2]2＋ （L = Pyridine or 4-methylpyridine（4-picoline）, bipy = 2,2＇-bipyridine, and 4,5-dimebip...New heteroleptic and homoleptic complexes of the type[Pd（4,5-dmbipy）C12], [Pd（4,5-dmbipy）L2], and [Pd（4,5-dimebipy）2]2＋ （L = Pyridine or 4-methylpyridine（4-picoline）, bipy = 2,2＇-bipyridine, and 4,5-dimebipy = 4,5-dimethyl-2,2＇-bipyridine） were synthesized and characterized by IH NMR and elemental analysis. The crystal structure of bis（4-methylpyridine）-4,5- dimethyl-2,2＇-bipyridinepalladium（II）perchlorate [Pd（4,5-dmbipy）（4-pic）2]（CIO4）2 was also determined by single crystal X-ray diffraction. This complex crystallized in the triclinic crystal system and space group PI with a = 9.562 （2）, b = 11.326 （4）, c = 15.0120 （10） A°; α = 70.940°, β= 77.60 （2）, γ= 67.86 （2） and z = 4. The Pd （II） in square planar environment showed a small distortion towards tetrahedral through one coordinated bipyridine ring twisting with respect to the other.展开更多
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 diffra...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.展开更多
There are several paths for synthesizing 4,4′ bis(hydroxymethyl) 2,2′ bipyridine, but most of them need strict experimental conditions that are not easy to be overcome. We designed a simple way to prepare this produ...There are several paths for synthesizing 4,4′ bis(hydroxymethyl) 2,2′ bipyridine, but most of them need strict experimental conditions that are not easy to be overcome. We designed a simple way to prepare this product via the oxidation of 4,4′ bismethyl 2,2′ bipyridine, followed by esterification and reduction. The yield increases and the reaction conditions become genial in contrast to those of other methods. The molecular structure of the final product was confirmed by means of elemental analysis, IR, 1H NMR and MS spectra.展开更多
文摘New heteroleptic and homoleptic complexes of the type[Pd（4,5-dmbipy）C12], [Pd（4,5-dmbipy）L2], and [Pd（4,5-dimebipy）2]2＋ （L = Pyridine or 4-methylpyridine（4-picoline）, bipy = 2,2＇-bipyridine, and 4,5-dimebipy = 4,5-dimethyl-2,2＇-bipyridine） were synthesized and characterized by IH NMR and elemental analysis. The crystal structure of bis（4-methylpyridine）-4,5- dimethyl-2,2＇-bipyridinepalladium（II）perchlorate [Pd（4,5-dmbipy）（4-pic）2]（CIO4）2 was also determined by single crystal X-ray diffraction. This complex crystallized in the triclinic crystal system and space group PI with a = 9.562 （2）, b = 11.326 （4）, c = 15.0120 （10） A°; α = 70.940°, β= 77.60 （2）, γ= 67.86 （2） and z = 4. The Pd （II） in square planar environment showed a small distortion towards tetrahedral through one coordinated bipyridine ring twisting with respect to the other.
基金This work was supported by the National Natural Science Foundation of China(No.20371028)Natural Science Foundation of Tianjin(No.023605811)
文摘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.
基金Supported by the National Natural Science Foundation of China(No. 2 0 16 2 0 0 5 ) the Foundation of EducationMinistry(No. 2 0 0 1- 3) .
文摘There are several paths for synthesizing 4,4′ bis(hydroxymethyl) 2,2′ bipyridine, but most of them need strict experimental conditions that are not easy to be overcome. We designed a simple way to prepare this product via the oxidation of 4,4′ bismethyl 2,2′ bipyridine, followed by esterification and reduction. The yield increases and the reaction conditions become genial in contrast to those of other methods. The molecular structure of the final product was confirmed by means of elemental analysis, IR, 1H NMR and MS spectra.
