The hydrothermal reaction of isonicotinic acid (4-C5H4N-COOH), Cu(ClO4)(2). 6H(2)O and water at 170 degreesC gave the title compound, [Cu(OH)(2)(H2O)(2)(4-C5H4N-COOH)(2)] (1), which was analyzed by single-crystal X-ra...The hydrothermal reaction of isonicotinic acid (4-C5H4N-COOH), Cu(ClO4)(2). 6H(2)O and water at 170 degreesC gave the title compound, [Cu(OH)(2)(H2O)(2)(4-C5H4N-COOH)(2)] (1), which was analyzed by single-crystal X-ray diffraction, The complex crystallizes in triclinic space group PY with unit cell parameters: a = 6.337(2), b = 6.894(3), c = 9.178(3). alpha = 99.40(3), beta = 105.26(3), gamma 108.17(5)degrees, V = 354.1(2)Angstrom (3), Z = 1, C12H16CuN2O8, M-r = 379.81, D-c = 1.791 Mg/m(3), F(000) 197, mu (MoK alpha) = 1.589 mm(-1). The final R and wR are 0.068 and 0.170 for 1249 observed reflections with I greater than or equal to2 sigma (I). The central copper ion is in a distorted octahedron geometry completed by two nitrogen atoms from carboxylic ligand, two oxygen atoms from hydroxyl groups and two oxygen atoms from coordinated water molecules. The intermolecular hydrogen bonding leads to the formation of a three-dimensional supramolecular structure.展开更多
Reaction of 2-pyridone, copper acetate and terbium(or yttrium) perchlorate in acetone with the mole ratio 6: 2: 1 results in the formation of heteronuclear complex Ln_2Cu_4L_8 (HL)_4 (OH)_2 (ClO_4)_4 (H_20)_(10) 2CH_3...Reaction of 2-pyridone, copper acetate and terbium(or yttrium) perchlorate in acetone with the mole ratio 6: 2: 1 results in the formation of heteronuclear complex Ln_2Cu_4L_8 (HL)_4 (OH)_2 (ClO_4)_4 (H_20)_(10) 2CH_3COCH_3(Ln = Tb (1), Y (2)). By recrystallizing (1) in CHCl_3 single crystals were obtained and the structure was determined by four-circle diffractometer. Data showed that the crystal is in space group C2/m with a=27. 454(9)A, b=13, 608A, c=30. 556(11)A, β=99. 89(3)°, v=11245. 7(7. 5)A^3. The structure was solved by a combination of Patterson method and Fourier technique. The final R value is 0. 103. In the structure, four copper and two terbium ions are bridged by 2-pyridone anions to form an essentially octahedral Cu_4Tb_2 core. The terbium atoms are each eight-coordinate and the copper atoms are five-coordinate.展开更多
The preparation of Cu nanoparticles by the aqueous solution reduction method was investigated. The effects of different reaction parameters on the preparation of Cu nanoparticles were studied. The optimum conditions f...The preparation of Cu nanoparticles by the aqueous solution reduction method was investigated. The effects of different reaction parameters on the preparation of Cu nanoparticles were studied. The optimum conditions for preparing well-dispersed nanoparticles were found as follows: 0.4 mol/L NaBH4 was added into solution containing 0.2 mol/L Cu2+, 1.0% gelatin dispersant in mass fraction, and 1.2 mol/L NH3?H2O at pH 12 and 313 K. In addition, a series of experiments were performed to discover the reaction process. NH3?H2O was found to be able to modulate the reaction process. At pH=10, Cu2+ was transformed to Cu(NH3)42+ as precursor after the addition of NH3?H2O, and then Cu(NH3)42+ was reduced by NaBH4 solution. At pH=12, Cu2+ was transformed to Cu(OH)2 as precursor after the addition of NH3?H2O, and Cu(OH)2 was then reduced by NaBH4 solution.展开更多
文摘The hydrothermal reaction of isonicotinic acid (4-C5H4N-COOH), Cu(ClO4)(2). 6H(2)O and water at 170 degreesC gave the title compound, [Cu(OH)(2)(H2O)(2)(4-C5H4N-COOH)(2)] (1), which was analyzed by single-crystal X-ray diffraction, The complex crystallizes in triclinic space group PY with unit cell parameters: a = 6.337(2), b = 6.894(3), c = 9.178(3). alpha = 99.40(3), beta = 105.26(3), gamma 108.17(5)degrees, V = 354.1(2)Angstrom (3), Z = 1, C12H16CuN2O8, M-r = 379.81, D-c = 1.791 Mg/m(3), F(000) 197, mu (MoK alpha) = 1.589 mm(-1). The final R and wR are 0.068 and 0.170 for 1249 observed reflections with I greater than or equal to2 sigma (I). The central copper ion is in a distorted octahedron geometry completed by two nitrogen atoms from carboxylic ligand, two oxygen atoms from hydroxyl groups and two oxygen atoms from coordinated water molecules. The intermolecular hydrogen bonding leads to the formation of a three-dimensional supramolecular structure.
基金Project supported by China National Climbing plan and National Nature Science Foundation
文摘Reaction of 2-pyridone, copper acetate and terbium(or yttrium) perchlorate in acetone with the mole ratio 6: 2: 1 results in the formation of heteronuclear complex Ln_2Cu_4L_8 (HL)_4 (OH)_2 (ClO_4)_4 (H_20)_(10) 2CH_3COCH_3(Ln = Tb (1), Y (2)). By recrystallizing (1) in CHCl_3 single crystals were obtained and the structure was determined by four-circle diffractometer. Data showed that the crystal is in space group C2/m with a=27. 454(9)A, b=13, 608A, c=30. 556(11)A, β=99. 89(3)°, v=11245. 7(7. 5)A^3. The structure was solved by a combination of Patterson method and Fourier technique. The final R value is 0. 103. In the structure, four copper and two terbium ions are bridged by 2-pyridone anions to form an essentially octahedral Cu_4Tb_2 core. The terbium atoms are each eight-coordinate and the copper atoms are five-coordinate.
文摘The preparation of Cu nanoparticles by the aqueous solution reduction method was investigated. The effects of different reaction parameters on the preparation of Cu nanoparticles were studied. The optimum conditions for preparing well-dispersed nanoparticles were found as follows: 0.4 mol/L NaBH4 was added into solution containing 0.2 mol/L Cu2+, 1.0% gelatin dispersant in mass fraction, and 1.2 mol/L NH3?H2O at pH 12 and 313 K. In addition, a series of experiments were performed to discover the reaction process. NH3?H2O was found to be able to modulate the reaction process. At pH=10, Cu2+ was transformed to Cu(NH3)42+ as precursor after the addition of NH3?H2O, and then Cu(NH3)42+ was reduced by NaBH4 solution. At pH=12, Cu2+ was transformed to Cu(OH)2 as precursor after the addition of NH3?H2O, and Cu(OH)2 was then reduced by NaBH4 solution.
