Crystals of sodium tridecafluorodizirconate Na5Zr2F13 were synthesized under mild hydrothermal conditions, and the structure was refined by single-crystal X-ray diffraction. The compound crystallizes in monoclinic wit...Crystals of sodium tridecafluorodizirconate Na5Zr2F13 were synthesized under mild hydrothermal conditions, and the structure was refined by single-crystal X-ray diffraction. The compound crystallizes in monoclinic with crystallographic data： Mr = 544.39, C2/m （No. 12）, a = 11.5600（9）, b = 5.4759（4）, c = 8.3989（6） A°, β = 97.361（10）°, V= 527.28（7） A°^3, Z= 2, Dc = 3.429 g/cm^3, 2 = 0.71073A° ,μ = 23.48 cm^-1, F（000） = 504, T= 295 K, Ri = 0.0173 and wR2 = 0.0449 for 55 variables and 682 contributing uniqUe reflections. The crystal structure is constituted with sixand eight-fold sodium atoms, forming irregular trigonal prisms and irregular cubes, respectively. Here, the zirconium atoms are connected with seven fluorine atoms to form a mono-capped trigonal prism. [Zr2F13]^5- complex ions formed by comer-shared [ZrF7]^3- are comer- and edgeshared to [Na4F22] and [Na3F8] cages, leading to the network structure. Thermal analysis, X-ray excited luminescence and photoluminescence under UV light measurements were conducted on Na5Zr2F13 crystals.展开更多
Complex(n-Bu_4N)[Mo_2O_2(OMe)(mp)_3][1,mp=(o-OC_(?)H_4S)^(2-)]was synthesized by the reaction of MoOCl_3(THF)_2 and Na_2mp in EtOH and crystallized in monoclinic space group P2_(?)/n with crystal data:a=13.910(3),b=23...Complex(n-Bu_4N)[Mo_2O_2(OMe)(mp)_3][1,mp=(o-OC_(?)H_4S)^(2-)]was synthesized by the reaction of MoOCl_3(THF)_2 and Na_2mp in EtOH and crystallized in monoclinic space group P2_(?)/n with crystal data:a=13.910(3),b=23.554(3),c=12.558(2)(?),β=105.20(2)°,Z=4,D_o=1.455g/ cm^3,final R=0.077 for 5325 reflections[I>3σ(I)].The two[Mo(O)mp]^+ moicties are bridged by one 1,2-bidentate ligand mp^(2-) with exceedingly small bite angle(69.0°)and bite distance (2.70(?))and by a methoxy group.The structure can be interpreted as two distorted octahedra around the Mo atoms sharing a face.Attempts have been made to provide structural informa- tions for the syntheses of modelling compounds of FeMoco by comparing the Mo—O and Mo—S bond distances of o-mercaptophenolate ligated compounds to those of the molybdenum site of nitrogenase.展开更多
The title compound, [{Na（H2O）3}2lRu（dmso）3}2（MoO4）3]·3H2O, has been obtained by the reaction of Na2MoO4·2H2O with cis-Ru（dmso）4Cl2 in aqueous solution. Its crystal structure was determined by single-...The title compound, [{Na（H2O）3}2lRu（dmso）3}2（MoO4）3]·3H2O, has been obtained by the reaction of Na2MoO4·2H2O with cis-Ru（dmso）4Cl2 in aqueous solution. Its crystal structure was determined by single-crystal X-ray diffraction method. The crystal crystallizes in the triclinic system, space group PI^- with a = 12.3333（3）, b = 12.6289（3）, c = 32.0284（14） A, α = 79.873（7）, β= 87.549（9）, γ = 64.500（4）°, V = 4429.5（2） A^3, Z = 4, Mr = 1358.85, Dc = 2.038 g/cm^3, F（000） = 2696 and μ = 1.874 mm^-1. The compound contains a novel pentanuclear triangle bipyramidal core, [{ Ru（dmso）3 } 2（MoO4）3]^2-, which consists of two { Ru（dmso）3 } ^2＋ fragments and three {μ2-MoO4}^2- units. Furthermore, the dmso ligands bridge the pentanuclear [Ru2Mo3] core and two [Na（H2O）3]^＋ fragments together, forming a neutral heptanuclear ruthenium- and sodiumcontaining polyoxomolybdate.展开更多
A novel and simple synthetic way using NaBH4 in the mixure of H2O-THF was applied to prepare 1,2-bis(diphenylphosphinoborane)ethane, dppe(BH3)2, in high yield and purity. The phosphanylborohydride compound dppe(BH3)2 ...A novel and simple synthetic way using NaBH4 in the mixure of H2O-THF was applied to prepare 1,2-bis(diphenylphosphinoborane)ethane, dppe(BH3)2, in high yield and purity. The phosphanylborohydride compound dppe(BH3)2 was isolated in the form of colorless crystals and characterized by single crystal X-ray diffraction, 1H, 13C, 31P and 11B NMR spectroscopy. Prismatic colorless crystals of dppe(BH3)2 were obtained in monoclinic crystal system and space group P21 with two asymmetric units in the unit cell. Lattice parameters were: a = 11.657(2), b = 17.237(2), c = 12.764(2) ?, β = 98.735(14)°, 2535.0(7) ?展开更多
Alluaudite-type NaMnV2(PO4)3 single crystal was successfully synthesized in the NaCl molten-salt media. The single-crystal diffraction data analysis shows that NaMnV2(PO4)3 crystallizes in monoclinic C2/c space group ...Alluaudite-type NaMnV2(PO4)3 single crystal was successfully synthesized in the NaCl molten-salt media. The single-crystal diffraction data analysis shows that NaMnV2(PO4)3 crystallizes in monoclinic C2/c space group with a = 12.098(2), b = 12.415(2), c = 6.4543(11)?, β = 114.614(2)°, V = 881.3(3) ?3, Mr = 464.64, Dc = 3.50158 g/cm3, μ(Mo Kα) = 4.046 mm-1, F(000) = 892.4 and Z = 2. The structure consists of MnO6, VO6 octahedra and PO4 tetrahedra, which form a three-dimensional architecture with two sets of large Na+ tunnels. The intercalation/deintercalation properties of NaMnV2(PO4)3 as positive and negative electrodes were tested in sodium batteries.展开更多
The title complex [CoIII(2, 2?bpy)2(N3)2]種O3?H2O was obtained by an auto-oxidization reaction of cobalt nitrate with 2, 2-bpy and sodium azide in aqueous solution at room temperature, and violet single crystals were ...The title complex [CoIII(2, 2?bpy)2(N3)2]種O3?H2O was obtained by an auto-oxidization reaction of cobalt nitrate with 2, 2-bpy and sodium azide in aqueous solution at room temperature, and violet single crystals were prepared in ethanol solution. The structure was determined by X-ray crystallography. The crystal is of triclinic, space group P ?with a = 8.285(4), b = 11.990(8), c = 12.596(7) ? a = 86.630(3), b = 86.280(5), g = 71.130(10)? C20H20CoN11O5, Mr = 553.40, Z = 2, V = 1180.6(12) ?, F(000) = 568, Dc = 1.557 g/cm3, m = 0.784 mm-1, R = 0.0403 and wR = 0.1008. The title complex consists of a [CoⅢ(2, 2?bpy)2(N3)2]+ cation, a NO3- anion and two lattice water molecules. The center CoⅢ ion coordinated by two chelating 2, 2?bpy ligands and two terminal azide groups with a CoN6 coordination environment exhibits a distorted octahedral geometry.展开更多
A homodinuclear complex （NH3CH2CH2CH2NH3）2 {Na2[（C6H4O2）2] （C6H4O2H）2} （1） has been synthesized by a solution-based self-assembly route. It crystallized in monoclinic system with space group P21/c. Every sodiu...A homodinuclear complex （NH3CH2CH2CH2NH3）2 {Na2[（C6H4O2）2] （C6H4O2H）2} （1） has been synthesized by a solution-based self-assembly route. It crystallized in monoclinic system with space group P21/c. Every sodium ion coordinates in a tetragonal prism fashion with two O atoms of a terminal chelating catecholate ligand and three O atoms from two bridging catecholate ligands. Two neighboring NaO5 tetragonal prisms are edge-shared and centrosymmetric with regard to the inversion center to form a binuclear cluster {Na2[（C6H4O2）2]（C6H4OOH）2}^4- anion. The complex anions were aligned parallelly by n-n interaction and linked with the protonated 1,3-propylenediamine through hydrogen bonds which were assembled into a multi-lamellar structure with channels. The crystal exhibits rectangular geometry with an interior triangle hollow structure under optical microscopy. And the scanning electron microscopy （SEM） indicates that the wall of the tubes shows multi-lamella morphologies. Further, the transmission electron microscopy （TEM） reveals that the crystal is composed of multi-lamellar nano-tubes with diameters less than 100 nm. The molecular structure of the complex was compared with that of its isomer complex 2.展开更多
基金This study was supported by the Fund from the key project from the NSF of China
文摘Crystals of sodium tridecafluorodizirconate Na5Zr2F13 were synthesized under mild hydrothermal conditions, and the structure was refined by single-crystal X-ray diffraction. The compound crystallizes in monoclinic with crystallographic data： Mr = 544.39, C2/m （No. 12）, a = 11.5600（9）, b = 5.4759（4）, c = 8.3989（6） A°, β = 97.361（10）°, V= 527.28（7） A°^3, Z= 2, Dc = 3.429 g/cm^3, 2 = 0.71073A° ,μ = 23.48 cm^-1, F（000） = 504, T= 295 K, Ri = 0.0173 and wR2 = 0.0449 for 55 variables and 682 contributing uniqUe reflections. The crystal structure is constituted with sixand eight-fold sodium atoms, forming irregular trigonal prisms and irregular cubes, respectively. Here, the zirconium atoms are connected with seven fluorine atoms to form a mono-capped trigonal prism. [Zr2F13]^5- complex ions formed by comer-shared [ZrF7]^3- are comer- and edgeshared to [Na4F22] and [Na3F8] cages, leading to the network structure. Thermal analysis, X-ray excited luminescence and photoluminescence under UV light measurements were conducted on Na5Zr2F13 crystals.
基金Project supported by the National Natural Science Foundation of Chinathe Natural Science Foundation of the Chinese Academy of Sciences the Natural Science Foundation of Fujian Province.
文摘Complex(n-Bu_4N)[Mo_2O_2(OMe)(mp)_3][1,mp=(o-OC_(?)H_4S)^(2-)]was synthesized by the reaction of MoOCl_3(THF)_2 and Na_2mp in EtOH and crystallized in monoclinic space group P2_(?)/n with crystal data:a=13.910(3),b=23.554(3),c=12.558(2)(?),β=105.20(2)°,Z=4,D_o=1.455g/ cm^3,final R=0.077 for 5325 reflections[I>3σ(I)].The two[Mo(O)mp]^+ moicties are bridged by one 1,2-bidentate ligand mp^(2-) with exceedingly small bite angle(69.0°)and bite distance (2.70(?))and by a methoxy group.The structure can be interpreted as two distorted octahedra around the Mo atoms sharing a face.Attempts have been made to provide structural informa- tions for the syntheses of modelling compounds of FeMoco by comparing the Mo—O and Mo—S bond distances of o-mercaptophenolate ligated compounds to those of the molybdenum site of nitrogenase.
基金This work was supported by the State Key Laboratory of Structural Chemistry, the National Ministry of Science and Technology of China(001CB1089), the NNSFC (20273073, 20333070 and 90206040) and NSF of Fujian Province (2003J042, 2004J041 and 2004HZ01-1)
文摘The title compound, [{Na（H2O）3}2lRu（dmso）3}2（MoO4）3]·3H2O, has been obtained by the reaction of Na2MoO4·2H2O with cis-Ru（dmso）4Cl2 in aqueous solution. Its crystal structure was determined by single-crystal X-ray diffraction method. The crystal crystallizes in the triclinic system, space group PI^- with a = 12.3333（3）, b = 12.6289（3）, c = 32.0284（14） A, α = 79.873（7）, β= 87.549（9）, γ = 64.500（4）°, V = 4429.5（2） A^3, Z = 4, Mr = 1358.85, Dc = 2.038 g/cm^3, F（000） = 2696 and μ = 1.874 mm^-1. The compound contains a novel pentanuclear triangle bipyramidal core, [{ Ru（dmso）3 } 2（MoO4）3]^2-, which consists of two { Ru（dmso）3 } ^2＋ fragments and three {μ2-MoO4}^2- units. Furthermore, the dmso ligands bridge the pentanuclear [Ru2Mo3] core and two [Na（H2O）3]^＋ fragments together, forming a neutral heptanuclear ruthenium- and sodiumcontaining polyoxomolybdate.
基金Partial support of this work by the Turkish Academy of Sciences and the Scientific and Technological Research Council of Turkey(TUBITAK,Project No:105M357)is gratefully acknowledgedL.T.Y ildirim thanks Hacettepe University Scientific Research Unit(grant,No.04 A602004)for financial support.
文摘A novel and simple synthetic way using NaBH4 in the mixure of H2O-THF was applied to prepare 1,2-bis(diphenylphosphinoborane)ethane, dppe(BH3)2, in high yield and purity. The phosphanylborohydride compound dppe(BH3)2 was isolated in the form of colorless crystals and characterized by single crystal X-ray diffraction, 1H, 13C, 31P and 11B NMR spectroscopy. Prismatic colorless crystals of dppe(BH3)2 were obtained in monoclinic crystal system and space group P21 with two asymmetric units in the unit cell. Lattice parameters were: a = 11.657(2), b = 17.237(2), c = 12.764(2) ?, β = 98.735(14)°, 2535.0(7) ?
基金supported by the Fund of Education Committee of Shaanxi Province(No.16JS103)the Natural Science Basic Research Plan in Shaanxi Province(No.2018JM2021)
文摘Alluaudite-type NaMnV2(PO4)3 single crystal was successfully synthesized in the NaCl molten-salt media. The single-crystal diffraction data analysis shows that NaMnV2(PO4)3 crystallizes in monoclinic C2/c space group with a = 12.098(2), b = 12.415(2), c = 6.4543(11)?, β = 114.614(2)°, V = 881.3(3) ?3, Mr = 464.64, Dc = 3.50158 g/cm3, μ(Mo Kα) = 4.046 mm-1, F(000) = 892.4 and Z = 2. The structure consists of MnO6, VO6 octahedra and PO4 tetrahedra, which form a three-dimensional architecture with two sets of large Na+ tunnels. The intercalation/deintercalation properties of NaMnV2(PO4)3 as positive and negative electrodes were tested in sodium batteries.
文摘The title complex [CoIII(2, 2?bpy)2(N3)2]種O3?H2O was obtained by an auto-oxidization reaction of cobalt nitrate with 2, 2-bpy and sodium azide in aqueous solution at room temperature, and violet single crystals were prepared in ethanol solution. The structure was determined by X-ray crystallography. The crystal is of triclinic, space group P ?with a = 8.285(4), b = 11.990(8), c = 12.596(7) ? a = 86.630(3), b = 86.280(5), g = 71.130(10)? C20H20CoN11O5, Mr = 553.40, Z = 2, V = 1180.6(12) ?, F(000) = 568, Dc = 1.557 g/cm3, m = 0.784 mm-1, R = 0.0403 and wR = 0.1008. The title complex consists of a [CoⅢ(2, 2?bpy)2(N3)2]+ cation, a NO3- anion and two lattice water molecules. The center CoⅢ ion coordinated by two chelating 2, 2?bpy ligands and two terminal azide groups with a CoN6 coordination environment exhibits a distorted octahedral geometry.
基金Project supported by the National Natural Science Foundation of China （No. 20271034） and the Natural Science Foundation of Beijing City （No. 2012005）.
文摘A homodinuclear complex （NH3CH2CH2CH2NH3）2 {Na2[（C6H4O2）2] （C6H4O2H）2} （1） has been synthesized by a solution-based self-assembly route. It crystallized in monoclinic system with space group P21/c. Every sodium ion coordinates in a tetragonal prism fashion with two O atoms of a terminal chelating catecholate ligand and three O atoms from two bridging catecholate ligands. Two neighboring NaO5 tetragonal prisms are edge-shared and centrosymmetric with regard to the inversion center to form a binuclear cluster {Na2[（C6H4O2）2]（C6H4OOH）2}^4- anion. The complex anions were aligned parallelly by n-n interaction and linked with the protonated 1,3-propylenediamine through hydrogen bonds which were assembled into a multi-lamellar structure with channels. The crystal exhibits rectangular geometry with an interior triangle hollow structure under optical microscopy. And the scanning electron microscopy （SEM） indicates that the wall of the tubes shows multi-lamella morphologies. Further, the transmission electron microscopy （TEM） reveals that the crystal is composed of multi-lamellar nano-tubes with diameters less than 100 nm. The molecular structure of the complex was compared with that of its isomer complex 2.
