Two organically templated uranium phosphites, （C4H12N）（UO2）（HPO3）（NO3） （Mr = 486.16） 1 and （C16H36N）2（UO2）2（H2PO3）2（HPO3）（NO3）2 （Mr= 1390.95） 2, were prepared by evaporation from aqueous solution...Two organically templated uranium phosphites, （C4H12N）（UO2）（HPO3）（NO3） （Mr = 486.16） 1 and （C16H36N）2（UO2）2（H2PO3）2（HPO3）（NO3）2 （Mr= 1390.95） 2, were prepared by evaporation from aqueous solution of uranyl nitrate, phosphite acid and their respective organic ammonium hydroxids. Their structures were determined by single-crystal X-ray diffraction and further characterized by infrared and fluorescence spectroscopy. In 1, pentagonal [UO7] bipyramids share comers with three [HPO3]2- tetrahedra and one edge with a [NO3]- anion to form [（UO2）- （HPO3）（NO3）]^- ladder-like chains parallel to the b axis. The structure of 2 is also based upon one-dimensional anionic [（UO2）2（H2PO3）2（HPO3）（NO3）2]2-chains of comer-sharing penta- gonal [UOT] bipyramids with [H2PO3]- and [HPO3] tetrahedra, which is still unknown in structural chemistry of uranium so far. Crystal data for 1： monoclinic, space group C2/m, a = 21.808（7）, b = 6.9605（15）, c = 8.357（2） A, β = 98.327（15）°, V= 1255.2（6） A^3, Z = 4, Dc = 2.573 g/cm^3, F（000） = 888, μ = 13.086 mm^-1 the final R = 0.0418 and wR = 0.0906 （I 〉 2σ（I））; and those for 2： monoclinic, space group C2/c, a = 36.4549（8）, b = 14.5296（11）, c = 20.8253（11） A, β = 101.7440（8）°, V= 10799.7（10） A3, Z = 8, Dc= 1.711 g/cm^3, F（000） = 5424,μ = 6.144 mm^-1, the final R= 0.0368 and wR= 0.0865 （I〉 2σ（I））.展开更多
The title compound has been synthesized by the reaction of(NH4)3VS4, CuBr and NMe4Br in pyridine and its structure was determined by singlecrystal X-ray diffraction. Crystallographic data: C40H40Br3Cu6N8S4V, M4= 1432....The title compound has been synthesized by the reaction of(NH4)3VS4, CuBr and NMe4Br in pyridine and its structure was determined by singlecrystal X-ray diffraction. Crystallographic data: C40H40Br3Cu6N8S4V, M4= 1432. 95,orthorhombic space group Fdd2, a= 29. 9519 (2), b=13. 4719 (2), c= 25. 8612 (4)A, V= 10435. 2 (4), Z= 8, Dc= 1.824 g/cm3, F(000)= 5616,μ(MoKa) =50.64 cm-1, the final R =0.091 and wR =0. 206 for those 3401 unique reflectionshaving . The crystal structure determination shows that the cluster consists of a tetrahedral VS4 core encapsulated by a distorted octahedral array of six copperatoms which have two different coordination geometries, trigonal and tetrahedral.展开更多
Catena-[bis (3-methyl-4-nitropyridine N-oxide ) cadmiumdichloride],[Cd(C_6H_6N_2O_3)_2Cl_2], M_r= 491. 56, monoclinic , P2_1, a= 3. 799 (3), b= 29. 231 ( 9),c=7. 679(5) A, β=100. 19(6)°, V=839. 4 A￣3, Z=2, D_c=...Catena-[bis (3-methyl-4-nitropyridine N-oxide ) cadmiumdichloride],[Cd(C_6H_6N_2O_3)_2Cl_2], M_r= 491. 56, monoclinic , P2_1, a= 3. 799 (3), b= 29. 231 ( 9),c=7. 679(5) A, β=100. 19(6)°, V=839. 4 A￣3, Z=2, D_c= 1. 94 g/cm￣3, λ(MoKa)= 0. 71069 A, F(000) =484, P(MoKa) = 16. 5 cm￣(-1), final R=0. 038 for 1202 Observed reflections, T= 296K. The Cd atom is octahedrally coordinated by two O atoms from the trans 3-methyl-4-nitropyridine N-oxide (pom) ligands in the axial positions and four Cl atoms lying in the equatorial plane. The coordination octahedra form chains along the short a axis by edge sharing through the Cl atoms.展开更多
文摘Two organically templated uranium phosphites, （C4H12N）（UO2）（HPO3）（NO3） （Mr = 486.16） 1 and （C16H36N）2（UO2）2（H2PO3）2（HPO3）（NO3）2 （Mr= 1390.95） 2, were prepared by evaporation from aqueous solution of uranyl nitrate, phosphite acid and their respective organic ammonium hydroxids. Their structures were determined by single-crystal X-ray diffraction and further characterized by infrared and fluorescence spectroscopy. In 1, pentagonal [UO7] bipyramids share comers with three [HPO3]2- tetrahedra and one edge with a [NO3]- anion to form [（UO2）- （HPO3）（NO3）]^- ladder-like chains parallel to the b axis. The structure of 2 is also based upon one-dimensional anionic [（UO2）2（H2PO3）2（HPO3）（NO3）2]2-chains of comer-sharing penta- gonal [UOT] bipyramids with [H2PO3]- and [HPO3] tetrahedra, which is still unknown in structural chemistry of uranium so far. Crystal data for 1： monoclinic, space group C2/m, a = 21.808（7）, b = 6.9605（15）, c = 8.357（2） A, β = 98.327（15）°, V= 1255.2（6） A^3, Z = 4, Dc = 2.573 g/cm^3, F（000） = 888, μ = 13.086 mm^-1 the final R = 0.0418 and wR = 0.0906 （I 〉 2σ（I））; and those for 2： monoclinic, space group C2/c, a = 36.4549（8）, b = 14.5296（11）, c = 20.8253（11） A, β = 101.7440（8）°, V= 10799.7（10） A3, Z = 8, Dc= 1.711 g/cm^3, F（000） = 5424,μ = 6.144 mm^-1, the final R= 0.0368 and wR= 0.0865 （I〉 2σ（I））.
文摘The title compound has been synthesized by the reaction of(NH4)3VS4, CuBr and NMe4Br in pyridine and its structure was determined by singlecrystal X-ray diffraction. Crystallographic data: C40H40Br3Cu6N8S4V, M4= 1432. 95,orthorhombic space group Fdd2, a= 29. 9519 (2), b=13. 4719 (2), c= 25. 8612 (4)A, V= 10435. 2 (4), Z= 8, Dc= 1.824 g/cm3, F(000)= 5616,μ(MoKa) =50.64 cm-1, the final R =0.091 and wR =0. 206 for those 3401 unique reflectionshaving . The crystal structure determination shows that the cluster consists of a tetrahedral VS4 core encapsulated by a distorted octahedral array of six copperatoms which have two different coordination geometries, trigonal and tetrahedral.
文摘Catena-[bis (3-methyl-4-nitropyridine N-oxide ) cadmiumdichloride],[Cd(C_6H_6N_2O_3)_2Cl_2], M_r= 491. 56, monoclinic , P2_1, a= 3. 799 (3), b= 29. 231 ( 9),c=7. 679(5) A, β=100. 19(6)°, V=839. 4 A￣3, Z=2, D_c= 1. 94 g/cm￣3, λ(MoKa)= 0. 71069 A, F(000) =484, P(MoKa) = 16. 5 cm￣(-1), final R=0. 038 for 1202 Observed reflections, T= 296K. The Cd atom is octahedrally coordinated by two O atoms from the trans 3-methyl-4-nitropyridine N-oxide (pom) ligands in the axial positions and four Cl atoms lying in the equatorial plane. The coordination octahedra form chains along the short a axis by edge sharing through the Cl atoms.
