A novel coordination polymer [Sm（4-Pyta）3（H2O）2]n has been synthesized by the hydrothermal reaction between 4-Pyta （4-Pyta = 4-pyridylthioacetate） and Sm（NO3）3. The structure was characterized by elemental ana...A novel coordination polymer [Sm（4-Pyta）3（H2O）2]n has been synthesized by the hydrothermal reaction between 4-Pyta （4-Pyta = 4-pyridylthioacetate） and Sm（NO3）3. The structure was characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space groupP1, with a = 9.100（2）, b = 11.842（3）, c = 12.183（3） A, α= 79.781（4）, β= 74.124（4）, γ = 841882（5）^o, V = 1241.6（5） A^3, Z = 2, Mr = 690.95, Dc = 1.84806 g/cm^3, F（000） = 686,μ = 2.669 mm^-1, the final R = 0.0388 and wR = 0.0808 for 4149 observed reflections with I 〉 2σ（I）. The structural analysis shows that the complex exhibits a one-dimensional architecture. Intermolecular hydrogen bonding interactions are found in the complex molecules.展开更多
Reactions of lanthanoid trichlorides with sodium cyclopentylcyclopentadienyl in THF afford bis(cyclopentylcyclopentadienyl) lanthanoid chloride complexes (C_5H_9C_5H_4)_2LnCl(THF)_n (Ln= Nd, Sm, n=1; Ln= Er, Yb, n= 0)...Reactions of lanthanoid trichlorides with sodium cyclopentylcyclopentadienyl in THF afford bis(cyclopentylcyclopentadienyl) lanthanoid chloride complexes (C_5H_9C_5H_4)_2LnCl(THF)_n (Ln= Nd, Sm, n=1; Ln= Er, Yb, n= 0). The compound [CP'_2SmCl(THF)]_2 (2) (Cp' =cyclopentylcy- clopentadienyl) crystallizes from mixed solvent of hexane and THF in monoclinic space group P_2_1/c with a = 11.583 (3), b = 23.019(6), c = 8.227 (2)(?), β= 90.26 (2)°, V= 2194 (1)(?)~3, D_c= 1.59 g/cm^3. μ= 28.6 cm^(-1), F(000) = 1060, Z= 2 (dimers). Its crystal molecule is a dimer with a crystallographic symmetry center. The central metal atom Sm is coordinated to two Cp' rings, two bridging chlorine atoms and one THF forming a distorted trigonal bipyramid. The crystal of [Cp'_2ErCl]_2 (3) belongs to the triclinic space group P(?) with a = 11.264 (2), b= 13.296(5), c = 14.296(6)(?), a = 96.99 (3), β= 112.47(2), γ= 102.78(2)°, V= 1865(1)(?)~3, D_c= 1.67 g /cm^3, μ= 48.0 cm^(-1), F(000) = 924, Z = 2 (dimers). The molecule is a dimer consisting of two Cp'_2 ErCl species bridged by two Cl atoms. The central metal atom Er is coordinated to two Cp' rings and two bridging chlorine atoms forming a pseudo- tetrahedron. All these complexes are soluble in THF, DME, Et_2O, toluene and hexane.展开更多
基金This work was supported by the Education Office of Anhui Province (No. 2003kj255)
文摘A novel coordination polymer [Sm（4-Pyta）3（H2O）2]n has been synthesized by the hydrothermal reaction between 4-Pyta （4-Pyta = 4-pyridylthioacetate） and Sm（NO3）3. The structure was characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space groupP1, with a = 9.100（2）, b = 11.842（3）, c = 12.183（3） A, α= 79.781（4）, β= 74.124（4）, γ = 841882（5）^o, V = 1241.6（5） A^3, Z = 2, Mr = 690.95, Dc = 1.84806 g/cm^3, F（000） = 686,μ = 2.669 mm^-1, the final R = 0.0388 and wR = 0.0808 for 4149 observed reflections with I 〉 2σ（I）. The structural analysis shows that the complex exhibits a one-dimensional architecture. Intermolecular hydrogen bonding interactions are found in the complex molecules.
文摘Reactions of lanthanoid trichlorides with sodium cyclopentylcyclopentadienyl in THF afford bis(cyclopentylcyclopentadienyl) lanthanoid chloride complexes (C_5H_9C_5H_4)_2LnCl(THF)_n (Ln= Nd, Sm, n=1; Ln= Er, Yb, n= 0). The compound [CP'_2SmCl(THF)]_2 (2) (Cp' =cyclopentylcy- clopentadienyl) crystallizes from mixed solvent of hexane and THF in monoclinic space group P_2_1/c with a = 11.583 (3), b = 23.019(6), c = 8.227 (2)(?), β= 90.26 (2)°, V= 2194 (1)(?)~3, D_c= 1.59 g/cm^3. μ= 28.6 cm^(-1), F(000) = 1060, Z= 2 (dimers). Its crystal molecule is a dimer with a crystallographic symmetry center. The central metal atom Sm is coordinated to two Cp' rings, two bridging chlorine atoms and one THF forming a distorted trigonal bipyramid. The crystal of [Cp'_2ErCl]_2 (3) belongs to the triclinic space group P(?) with a = 11.264 (2), b= 13.296(5), c = 14.296(6)(?), a = 96.99 (3), β= 112.47(2), γ= 102.78(2)°, V= 1865(1)(?)~3, D_c= 1.67 g /cm^3, μ= 48.0 cm^(-1), F(000) = 924, Z = 2 (dimers). The molecule is a dimer consisting of two Cp'_2 ErCl species bridged by two Cl atoms. The central metal atom Er is coordinated to two Cp' rings and two bridging chlorine atoms forming a pseudo- tetrahedron. All these complexes are soluble in THF, DME, Et_2O, toluene and hexane.
