A new dicopper(II) compound with oxalate and reduced imino nitroxide radicals [Cu2(m-C2O4)(Him2-py)2(H2O)2](NO3)2 (Him2-py=1-hydroxy-2-(2-pyridyl)-4,4,5,5-tetramethyli- midazoline) has been synthesized and its crystal...A new dicopper(II) compound with oxalate and reduced imino nitroxide radicals [Cu2(m-C2O4)(Him2-py)2(H2O)2](NO3)2 (Him2-py=1-hydroxy-2-(2-pyridyl)-4,4,5,5-tetramethyli- midazoline) has been synthesized and its crystal structure was determined by X-ray diffraction method. The complex crystallizes in monoclinic, space group P21/n with a = 9.913(4), b = 19.057(8), c = 10.169(4) ? b = 114.292(7), V = 1751(1) 3, C26H38Cu2N8O14, Mr = 813.72, Dc = 1.543 g/cm3, m(MoKa) = 1.290 mm-1, F(000) = 840, Z = 2, the final R = 0.0398 and wR = 0.0986 for 1878 observed reflections (I>2s(I)). The imino nitroxide 2-(2-pyridyl)-4,4,5,5-tetramethyl- imidazoline-1-oxyl (im2-py) is reduced in the reaction to yield Him2-py which consists of oxalato-bridged centrosymmetric [Cu2(m-C2O4)(Him2-py)2(H2O)2]2+ ions and noncoordinated NO3- anions. Each copper(II) ion is in a distorted tetragonal pyramid environment: two nitrogen atoms from Him2-py and two oxygen atoms from the oxalate group are in the basal plane, and one water molecule at the axial position.展开更多
The title compound [Cu(Phen)3](ClO4)2(btio)(H2O), where btio = 2-(4- benzoyloxyl)-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide, has been prepared and structurally characterized by X-ray diffraction. It crystallizes i...The title compound [Cu(Phen)3](ClO4)2(btio)(H2O), where btio = 2-(4- benzoyloxyl)-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide, has been prepared and structurally characterized by X-ray diffraction. It crystallizes in triclinic, space group P?with a = 13.049(4), b = 13.827(5), c = 14.860(5) , a = 71.736(6), b = 77.076(6), g = 87.054(6)? C50H43Cl2CuN8O13, Mr = 1098.36, V = 2481(1) 3, Z = 2, Dc = 1.470 g/cm3, m(MoKa) = 0.622 mm-1, F(000) = 1132, the final R = 0.0639 and wR = 0.1473 for 8705 independent reflections with Rint =0.0285. The title compound is composed of [Cu(Phen)3]2+ moiety , one btio, two perchlorate ions and one water molecule. The copper(II) ion is octahedrally coordinated by three 1,10-phenanthroline ligands. The outer sphere consisting of one btio, two perchlorate ions and one water molecule is combined with the inner by hydrogen bonds and electrostatic interactions.展开更多
A novel complex [Ag(NIT3Py)3]?(ClO4)(H2O) has been synthesized and structurally characterized by X-ray diffraction method. It crystallizes in the rhombohedral system, space group R 3 with a = 15.8227(17), b = 15.8227(...A novel complex [Ag(NIT3Py)3]?(ClO4)(H2O) has been synthesized and structurally characterized by X-ray diffraction method. It crystallizes in the rhombohedral system, space group R 3 with a = 15.8227(17), b = 15.8227(17), c = 31.445(3) ?, γ = 120°, V = 6817.8(12) ?3, Dc = 1.370 g/cm3, Z = 6, μ = 0.566 mm-1, Mr = 937.18, F(000) = 2916, R = 0.0715, wR = 0.2115 and GOF = 1.086. The structure consists of Ag(NIT3Py)3+ cation moiety, one water molecule and one perchloric ion. The Ag(I) ion is in a trigonal planar coordination environment formed by three nitrogen atoms from three NIT3Py ligand molecules.展开更多
The title complexes [CoⅢ(TPA)(N3)2](ClO4) 1 and [CuⅡ(TPA)(N3)](ClO4) 2 have been synthesized and characterized by single-crystal X-ray diffraction. The crystal of 1 is of monoclinic, space group P21/n with a = 10.73...The title complexes [CoⅢ(TPA)(N3)2](ClO4) 1 and [CuⅡ(TPA)(N3)](ClO4) 2 have been synthesized and characterized by single-crystal X-ray diffraction. The crystal of 1 is of monoclinic, space group P21/n with a = 10.734(3), b = 13.112(4), c = 15.327(4) , = 93.023(6), V = 2154.2(11) ?, Mr = 532.80, Z = 4, Dc = 1.643 g/cm3, m(MoKa) = 0.71073 ? F(000) = 1088, R = 0.0502 and wR = 0.0928. The CoⅢ atom is coordinated by one chelating TPA ligand and two terminal azide groups to form a distorted octahedral geometry. The crystal of 2 belongs to monoclinic, space group P21/c with a = 15.405(6), b = 9.269(4), c = 14.998(6) 3, = 93.489(7), V = 2137.6(14) ? Mr = 495.38, Z = 4, Dc = 1.539 g/cm3, m(MoKa ) = 0.71073 ? F(000) = 1012, R = 0.0521 and wR = 0.0992. The CuⅡ atom is coordinated by one chelating TPA ligand and one terminal azide group, forming a distorted trigonal bipyramidal geometry.展开更多
基金This work was supported by the National Natural Science Foundation of China (No. 20271029)
文摘A new dicopper(II) compound with oxalate and reduced imino nitroxide radicals [Cu2(m-C2O4)(Him2-py)2(H2O)2](NO3)2 (Him2-py=1-hydroxy-2-(2-pyridyl)-4,4,5,5-tetramethyli- midazoline) has been synthesized and its crystal structure was determined by X-ray diffraction method. The complex crystallizes in monoclinic, space group P21/n with a = 9.913(4), b = 19.057(8), c = 10.169(4) ? b = 114.292(7), V = 1751(1) 3, C26H38Cu2N8O14, Mr = 813.72, Dc = 1.543 g/cm3, m(MoKa) = 1.290 mm-1, F(000) = 840, Z = 2, the final R = 0.0398 and wR = 0.0986 for 1878 observed reflections (I>2s(I)). The imino nitroxide 2-(2-pyridyl)-4,4,5,5-tetramethyl- imidazoline-1-oxyl (im2-py) is reduced in the reaction to yield Him2-py which consists of oxalato-bridged centrosymmetric [Cu2(m-C2O4)(Him2-py)2(H2O)2]2+ ions and noncoordinated NO3- anions. Each copper(II) ion is in a distorted tetragonal pyramid environment: two nitrogen atoms from Him2-py and two oxygen atoms from the oxalate group are in the basal plane, and one water molecule at the axial position.
基金This work was supported by the National Natural Science Foundation of China (No. 20171025 and No. 20331010)
文摘The title compound [Cu(Phen)3](ClO4)2(btio)(H2O), where btio = 2-(4- benzoyloxyl)-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide, has been prepared and structurally characterized by X-ray diffraction. It crystallizes in triclinic, space group P?with a = 13.049(4), b = 13.827(5), c = 14.860(5) , a = 71.736(6), b = 77.076(6), g = 87.054(6)? C50H43Cl2CuN8O13, Mr = 1098.36, V = 2481(1) 3, Z = 2, Dc = 1.470 g/cm3, m(MoKa) = 0.622 mm-1, F(000) = 1132, the final R = 0.0639 and wR = 0.1473 for 8705 independent reflections with Rint =0.0285. The title compound is composed of [Cu(Phen)3]2+ moiety , one btio, two perchlorate ions and one water molecule. The copper(II) ion is octahedrally coordinated by three 1,10-phenanthroline ligands. The outer sphere consisting of one btio, two perchlorate ions and one water molecule is combined with the inner by hydrogen bonds and electrostatic interactions.
基金This work was supported by the National Natural Science Foundation of China (No. 20331010) and Natural Science Foundation (No.033602011) of Tianjin
文摘A novel complex [Ag(NIT3Py)3]?(ClO4)(H2O) has been synthesized and structurally characterized by X-ray diffraction method. It crystallizes in the rhombohedral system, space group R 3 with a = 15.8227(17), b = 15.8227(17), c = 31.445(3) ?, γ = 120°, V = 6817.8(12) ?3, Dc = 1.370 g/cm3, Z = 6, μ = 0.566 mm-1, Mr = 937.18, F(000) = 2916, R = 0.0715, wR = 0.2115 and GOF = 1.086. The structure consists of Ag(NIT3Py)3+ cation moiety, one water molecule and one perchloric ion. The Ag(I) ion is in a trigonal planar coordination environment formed by three nitrogen atoms from three NIT3Py ligand molecules.
基金Supported by the National Natural Science Foundation of China (No. 20171026) and Natural Science Foundation of Tianjin (No. 013605811)
文摘The title complexes [CoⅢ(TPA)(N3)2](ClO4) 1 and [CuⅡ(TPA)(N3)](ClO4) 2 have been synthesized and characterized by single-crystal X-ray diffraction. The crystal of 1 is of monoclinic, space group P21/n with a = 10.734(3), b = 13.112(4), c = 15.327(4) , = 93.023(6), V = 2154.2(11) ?, Mr = 532.80, Z = 4, Dc = 1.643 g/cm3, m(MoKa) = 0.71073 ? F(000) = 1088, R = 0.0502 and wR = 0.0928. The CoⅢ atom is coordinated by one chelating TPA ligand and two terminal azide groups to form a distorted octahedral geometry. The crystal of 2 belongs to monoclinic, space group P21/c with a = 15.405(6), b = 9.269(4), c = 14.998(6) 3, = 93.489(7), V = 2137.6(14) ? Mr = 495.38, Z = 4, Dc = 1.539 g/cm3, m(MoKa ) = 0.71073 ? F(000) = 1012, R = 0.0521 and wR = 0.0992. The CuⅡ atom is coordinated by one chelating TPA ligand and one terminal azide group, forming a distorted trigonal bipyramidal geometry.
