A novel palladium(II) complex [(TMEDA)Pd(anca)2].2DMSO (1, TMEDA = N,N,N',N'-tetramethylethylethylenediamine, anca = anthracene-9-carboxylic acid) was synthesized and characterized by single-crystal X-ray di...A novel palladium(II) complex [(TMEDA)Pd(anca)2].2DMSO (1, TMEDA = N,N,N',N'-tetramethylethylethylenediamine, anca = anthracene-9-carboxylic acid) was synthesized and characterized by single-crystal X-ray diffraction, 1H NMR, UV-Vis and fluorescence spectroscopy. The cell belongs to orthorhombic Aba2 space group with a = 19.698(7), b = 21.045(7) c = 9.062(3) A, Z = 4, V= 3757(2) A3, C40H46N206PdS2, Mr = 821.31, D, = 1.452 g/cm3, F(000) = 1704, the final R = 0.0272, wR = 0.0667 and GOOF = 0.999. Complex 1 exhibits an interesting distorted clip-shaped molecular configuration which is stabilized by intramolecular C-H...O hydrogen bonds. The cells are packed into a 3D supramolecular structure based on the intermolecular C-H...zr interactions which further construct the tubular channels serving as guest molecular channels to include the DMSO solvent molecules inside. Furthermore, the spectroscopic properties of 1 were also investigated.展开更多
By employing the dithiocarbamate salt (K(PPDC), where PPDC = 4?-pyridyl-1-pipe-razine-4-dithiocarbamate) as the functional ligand and di-palladium complexes [(N^N)2Pd2(NO3ˉ)2](NO3ˉ)2 (N^N = 2,2'-bipyri...By employing the dithiocarbamate salt (K(PPDC), where PPDC = 4?-pyridyl-1-pipe-razine-4-dithiocarbamate) as the functional ligand and di-palladium complexes [(N^N)2Pd2(NO3ˉ)2](NO3ˉ)2 (N^N = 2,2'-bipyridine, bpy; 4,4'-dimethylbipyridine, dmbpy) as corner, two novel single metal complexes with Pd(II) centers have been obtained. These organic-metal complexes were characterized by NMR, ESI-MS, elemental analysis, Uv-vis spectra and single-crystal X-ray diffraction analysis. Compound 1?(PF6)2 ([(bpy)Pd(PPDC)]·(PF6)2) crystallizes in triclinic, space group P , a = 8.3968(5), b = 11.5565(7), c = 18.2234(11), α = 97.505(1), β = 91.424(1), γ = 106.146(1)o, C22H24N6S2P2F12Pd, Mr = 832.93, V = 1680.58(18) ?3, Z = 2, Dc = 1.646 Mg/m3, μ(MoKα) = 0.863 mm-1, F(000) = 828, the final R = 0.0455 and wR = 0.1390 for 6981 observed reflections with I 〉 2σ(I). Similarly, compound 2?(PF6)2 ([(dmbpy)Pd(PPDC)]·(PF6)2) also crystallizes in triclinic, space group P , a = 13.9467(3), b = 14.8390(2), c = 17.0632(3) ?, α = 81.8680(10), β = 87.051(2), γ = 83.4590(10)o, C22H25N5S2P2F12Pd, Mr = 819.93, V = 3470.81(11) ?3, Z = 4, Dc = 1.569 Mg/m3, μ(CuKα) = 7.115 mm-1, F(000) = 1632, the final R = 0.0606 and wR = 0.1637 for 12835 observed reflections with I 〉 2σ(I). Crystallography reveals that each metal center coordinates with two N atoms from bpy and two S atoms from PPDC in the square coordination mode. In the crystal structure of complex 1, a weak Pd……Pd interaction can be observed. Interestingly, it was also found that the mononuclear moieties of complex 2 could be packed into a 3-D porous framework via multiple intermolecular C–F……H hydrogen-boding interactions which extended in the a, b, and c axes with PF6ˉ anions frozen inside.展开更多
基金supported by the National Natural Science Foundation of China (No.91127039, 21471011)the Importation and Development of HighCaliber Talents Project of Beijing Municipal Institution~~
基金supported by the National Natural Science Foundation of China(No.91127039,51073171)Natural Science Foundation of Beijing(No.2112018)
文摘A novel palladium(II) complex [(TMEDA)Pd(anca)2].2DMSO (1, TMEDA = N,N,N',N'-tetramethylethylethylenediamine, anca = anthracene-9-carboxylic acid) was synthesized and characterized by single-crystal X-ray diffraction, 1H NMR, UV-Vis and fluorescence spectroscopy. The cell belongs to orthorhombic Aba2 space group with a = 19.698(7), b = 21.045(7) c = 9.062(3) A, Z = 4, V= 3757(2) A3, C40H46N206PdS2, Mr = 821.31, D, = 1.452 g/cm3, F(000) = 1704, the final R = 0.0272, wR = 0.0667 and GOOF = 0.999. Complex 1 exhibits an interesting distorted clip-shaped molecular configuration which is stabilized by intramolecular C-H...O hydrogen bonds. The cells are packed into a 3D supramolecular structure based on the intermolecular C-H...zr interactions which further construct the tubular channels serving as guest molecular channels to include the DMSO solvent molecules inside. Furthermore, the spectroscopic properties of 1 were also investigated.
基金supported by the National Natural Science Foundation of China(No.21471011)High-caliber Talents Project of Beijing Municipal Institution
文摘By employing the dithiocarbamate salt (K(PPDC), where PPDC = 4?-pyridyl-1-pipe-razine-4-dithiocarbamate) as the functional ligand and di-palladium complexes [(N^N)2Pd2(NO3ˉ)2](NO3ˉ)2 (N^N = 2,2'-bipyridine, bpy; 4,4'-dimethylbipyridine, dmbpy) as corner, two novel single metal complexes with Pd(II) centers have been obtained. These organic-metal complexes were characterized by NMR, ESI-MS, elemental analysis, Uv-vis spectra and single-crystal X-ray diffraction analysis. Compound 1?(PF6)2 ([(bpy)Pd(PPDC)]·(PF6)2) crystallizes in triclinic, space group P , a = 8.3968(5), b = 11.5565(7), c = 18.2234(11), α = 97.505(1), β = 91.424(1), γ = 106.146(1)o, C22H24N6S2P2F12Pd, Mr = 832.93, V = 1680.58(18) ?3, Z = 2, Dc = 1.646 Mg/m3, μ(MoKα) = 0.863 mm-1, F(000) = 828, the final R = 0.0455 and wR = 0.1390 for 6981 observed reflections with I 〉 2σ(I). Similarly, compound 2?(PF6)2 ([(dmbpy)Pd(PPDC)]·(PF6)2) also crystallizes in triclinic, space group P , a = 13.9467(3), b = 14.8390(2), c = 17.0632(3) ?, α = 81.8680(10), β = 87.051(2), γ = 83.4590(10)o, C22H25N5S2P2F12Pd, Mr = 819.93, V = 3470.81(11) ?3, Z = 4, Dc = 1.569 Mg/m3, μ(CuKα) = 7.115 mm-1, F(000) = 1632, the final R = 0.0606 and wR = 0.1637 for 12835 observed reflections with I 〉 2σ(I). Crystallography reveals that each metal center coordinates with two N atoms from bpy and two S atoms from PPDC in the square coordination mode. In the crystal structure of complex 1, a weak Pd……Pd interaction can be observed. Interestingly, it was also found that the mononuclear moieties of complex 2 could be packed into a 3-D porous framework via multiple intermolecular C–F……H hydrogen-boding interactions which extended in the a, b, and c axes with PF6ˉ anions frozen inside.