A new compound, (H3O)3{Na3(H2O)13(Cu(Gly)2)2(H2W12O42)}·11H2O (1), has been synthesized and structurally characterized, which represents the first example of a polyoxotungstate-surface being decorated with amino ...A new compound, (H3O)3{Na3(H2O)13(Cu(Gly)2)2(H2W12O42)}·11H2O (1), has been synthesized and structurally characterized, which represents the first example of a polyoxotungstate-surface being decorated with amino acid ligand. Two cis-{Cu(Gly)2}2+ engraft into the (H2W12O42)10- with Cu-O bond of 0.241 2(7) nm, and Na+ ions linked these (Cu(Gly)2)2(H2W12O42)6- clusters into a one-dimensional chain. CCDC: 278000.展开更多
A binuclear vanadium complex NH4[(VⅣO)2( Ⅲ(H2O)9] wa s synthesized by reaction of NH3VO3, nitrilotriacetic acid and EuCl3 in one aque ous solution. The crystal X-ray analysis shows that the complex contains one bin ...A binuclear vanadium complex NH4[(VⅣO)2( Ⅲ(H2O)9] wa s synthesized by reaction of NH3VO3, nitrilotriacetic acid and EuCl3 in one aque ous solution. The crystal X-ray analysis shows that the complex contains one bin uclear vanadium anion [(VⅣO)2( -and one [EuⅢ(H2O)9]3+ cation. T he molecules are built up to a three-dimensional supramolecular structure throug h hydrogen bonding. CCDC: 238716.展开更多
[{Cu(phen)(DMF)2}2(β-Mo8O26)] 1 (C36H44Cu2Mo8N8O30, Mr = 1963.39, phen =- 1,10-phenanthroline) and [Cu(phen)2]2[{Cu(phen)}2Mo8O26] 2 (C72H48Cu4Mo8N12O26, Mr = 2518.90) have been synthesized from (Bu4N...[{Cu(phen)(DMF)2}2(β-Mo8O26)] 1 (C36H44Cu2Mo8N8O30, Mr = 1963.39, phen =- 1,10-phenanthroline) and [Cu(phen)2]2[{Cu(phen)}2Mo8O26] 2 (C72H48Cu4Mo8N12O26, Mr = 2518.90) have been synthesized from (Bu4N)2[Mo6O19], Cu(NO3)2·3H2O and phen using solution method and under solvothermal condition, respectively. Both compounds 1 and 2 are structurally characterized by elemental analyses, IR and single-crystal X-ray diffraction. Compound 1 crystallizes in the monoclinic system, space group P21/n, with a = 16.3347(13), b = 9.861(1), c = 17.2827(14) A, β=99.099(4)°, V= 2748.8(3) A3, Z = 2, Dc= 2.372 g/cm^3, F(000) =1900 and μ= 2.614 mm^-1. X-ray diffraction analysis reveals that compound 1 consists of discrete {[Cu(phen)(DMF)2]2(β-Mo8O26)} clusters constructed from β-[Mo8O26]^4- subunits covalently bound to two [Cu(phen)(DMF)2]^2- coordination groups. Compound 2 crystallizes in the monoclinic system, space group C2/c, with a = 33.1401(9), b = 16.4508(5), c = 16.2622(4) A, β= 119.2460(10)°, V = 7735.7(4) A3, Z = 4, Dc = 2.163 g/cm^3, F(000) = 4896 and μ= 2.413mm^-1. X-ray diffraction analysis reveals that compound 2 consists of a centrosymmetric β-octamolybdate-supported complex anion [ {Cu(phen)}2Mo8O26] and two bis-phenanthroline Cu(I) cations.展开更多
Cobalt-based phosphate/phosphonates are a class of promising water oxidation catalysts at neutralpH.Herein,we reported a facile hydrothermal synthesis of various nanostructured cobalt phe-nylphosphonates.It is found t...Cobalt-based phosphate/phosphonates are a class of promising water oxidation catalysts at neutralpH.Herein,we reported a facile hydrothermal synthesis of various nanostructured cobalt phe-nylphosphonates.It is found that the number of hydroxyl group of structure-directing reagent iscrucial for the construction of 3D hierarchical structures including hierarchical nanosheet flow-er-like assemblies and nanothorn microsphere.These samples were characterized by scanningelectron microscopy,transmission electron microscopy,X-ray diffraction,infrared,and X-ray pho-toelectron spectroscopy techniques.They can act as highly efficient electrocatalysts for the oxygenevolution reaction at neutral pH.Among these,hierarchical cobalt phenylphosphonate nanothornflowers present excellent performance,affording a current density of 1 mA cm^-2 required a smalloverpotential of 393 mV.This work offers a new clue to develop high-performance metal phospho-nate/phosphate catalysts toward electrochemical water oxidation.展开更多
The crystals of the title compounds (H3O)(C3H5N2)[Mn(OH)6Mo6O18]?3.5H2O 1 and (H3O)3[Co(OH)6Mo6O18]?7H2O 2 have been prepared and structurally determined by X-ray single-crystal diffraction. Compound 1 crystallizes ...The crystals of the title compounds (H3O)(C3H5N2)[Mn(OH)6Mo6O18]?3.5H2O 1 and (H3O)3[Co(OH)6Mo6O18]?7H2O 2 have been prepared and structurally determined by X-ray single-crystal diffraction. Compound 1 crystallizes in monoclinic, space group C2/c with a = 21.5018(9), b = 10.9331(5), c = 11.8667(5) ?, β = 95.3570(10)o, V = 2777.5(2) ?3, Z = 4, Dc = 2.802 g/cm3, Mr = 1171.80, μ(MoKα) = 3.173 mm-1, F(000) = 223, the final R = 0.0458 and wR = 0.1041 for 2093 observed reflections (I > 2σ(I)); Compound 2 crystallizes in monoclinic, space group P21/c with a = 11.4042(12), b = 10.9481(11), c = 11.6722(12) ?, β = 99.948(2)o, V = 1435.4(3) ?3, Z = 2, Dc = 2.794 g/cm3, Mr = 1207.80, μ(MoKα) = 3.223 mm-1, F(000) = 1160, the final R = 0.0544 and wR = 0.1066 for 1906 observed reflections (I > 2σ(I)). Both compounds 1 and 2 adopt the Anderson structure, in which the anion is of centrosymmetry and formed by six octahedral edge-sharing MoO6units surrounding the central MO6 (M = Mn or Co) octahedron.展开更多
The title compound, {Mn(H2O)4(VO)2(PO4)2}n 1, was synthesized by the hydro- thermal reaction of Mn(OAc)2, Na2VO3 and H3PO4 in aqueous solution and its crystal structure was determined by X-ray single-crystal analysi...The title compound, {Mn(H2O)4(VO)2(PO4)2}n 1, was synthesized by the hydro- thermal reaction of Mn(OAc)2, Na2VO3 and H3PO4 in aqueous solution and its crystal structure was determined by X-ray single-crystal analysis. Crystallographic data for 1: H4MnO14P2V2, tetragonal system, space group I4/mmm, a = 6.251(3), c = 13.410(9) ?, Mr = 446.79, V = 524.0(5) ?3, Z = 2, F(000) = 434, μ = 3.320 mm-1, Dc = 2.832 g/cm3, the final R = 0.0577 for 163 observed reflections (I > 2σ(I)). X-ray crystal structure analysis shows that the vanadium phosphorous oxide layers are further connected by MnII(H2O)4 cations to form a three-dimensional network.展开更多
文摘A new compound, (H3O)3{Na3(H2O)13(Cu(Gly)2)2(H2W12O42)}·11H2O (1), has been synthesized and structurally characterized, which represents the first example of a polyoxotungstate-surface being decorated with amino acid ligand. Two cis-{Cu(Gly)2}2+ engraft into the (H2W12O42)10- with Cu-O bond of 0.241 2(7) nm, and Na+ ions linked these (Cu(Gly)2)2(H2W12O42)6- clusters into a one-dimensional chain. CCDC: 278000.
文摘A binuclear vanadium complex NH4[(VⅣO)2( Ⅲ(H2O)9] wa s synthesized by reaction of NH3VO3, nitrilotriacetic acid and EuCl3 in one aque ous solution. The crystal X-ray analysis shows that the complex contains one bin uclear vanadium anion [(VⅣO)2( -and one [EuⅢ(H2O)9]3+ cation. T he molecules are built up to a three-dimensional supramolecular structure throug h hydrogen bonding. CCDC: 238716.
基金This work was supported by the 973 Program of the MOST (001CB108906), the National Natural Science Foundation of China (90206040, 20425313, 20333070, 20521101, and 20303021), the Natural Science Foundation of Fujian Province (2005HZ01-1), and the Chinese Academy of Sciences
文摘[{Cu(phen)(DMF)2}2(β-Mo8O26)] 1 (C36H44Cu2Mo8N8O30, Mr = 1963.39, phen =- 1,10-phenanthroline) and [Cu(phen)2]2[{Cu(phen)}2Mo8O26] 2 (C72H48Cu4Mo8N12O26, Mr = 2518.90) have been synthesized from (Bu4N)2[Mo6O19], Cu(NO3)2·3H2O and phen using solution method and under solvothermal condition, respectively. Both compounds 1 and 2 are structurally characterized by elemental analyses, IR and single-crystal X-ray diffraction. Compound 1 crystallizes in the monoclinic system, space group P21/n, with a = 16.3347(13), b = 9.861(1), c = 17.2827(14) A, β=99.099(4)°, V= 2748.8(3) A3, Z = 2, Dc= 2.372 g/cm^3, F(000) =1900 and μ= 2.614 mm^-1. X-ray diffraction analysis reveals that compound 1 consists of discrete {[Cu(phen)(DMF)2]2(β-Mo8O26)} clusters constructed from β-[Mo8O26]^4- subunits covalently bound to two [Cu(phen)(DMF)2]^2- coordination groups. Compound 2 crystallizes in the monoclinic system, space group C2/c, with a = 33.1401(9), b = 16.4508(5), c = 16.2622(4) A, β= 119.2460(10)°, V = 7735.7(4) A3, Z = 4, Dc = 2.163 g/cm^3, F(000) = 4896 and μ= 2.413mm^-1. X-ray diffraction analysis reveals that compound 2 consists of a centrosymmetric β-octamolybdate-supported complex anion [ {Cu(phen)}2Mo8O26] and two bis-phenanthroline Cu(I) cations.
文摘Cobalt-based phosphate/phosphonates are a class of promising water oxidation catalysts at neutralpH.Herein,we reported a facile hydrothermal synthesis of various nanostructured cobalt phe-nylphosphonates.It is found that the number of hydroxyl group of structure-directing reagent iscrucial for the construction of 3D hierarchical structures including hierarchical nanosheet flow-er-like assemblies and nanothorn microsphere.These samples were characterized by scanningelectron microscopy,transmission electron microscopy,X-ray diffraction,infrared,and X-ray pho-toelectron spectroscopy techniques.They can act as highly efficient electrocatalysts for the oxygenevolution reaction at neutral pH.Among these,hierarchical cobalt phenylphosphonate nanothornflowers present excellent performance,affording a current density of 1 mA cm^-2 required a smalloverpotential of 393 mV.This work offers a new clue to develop high-performance metal phospho-nate/phosphate catalysts toward electrochemical water oxidation.
基金This work was supported by the National Natural Science Foundation of China (90206040 20333070and 20303021) and Natural Science Foundation of Fujian Province (20002F015 and 2002J006)
文摘The crystals of the title compounds (H3O)(C3H5N2)[Mn(OH)6Mo6O18]?3.5H2O 1 and (H3O)3[Co(OH)6Mo6O18]?7H2O 2 have been prepared and structurally determined by X-ray single-crystal diffraction. Compound 1 crystallizes in monoclinic, space group C2/c with a = 21.5018(9), b = 10.9331(5), c = 11.8667(5) ?, β = 95.3570(10)o, V = 2777.5(2) ?3, Z = 4, Dc = 2.802 g/cm3, Mr = 1171.80, μ(MoKα) = 3.173 mm-1, F(000) = 223, the final R = 0.0458 and wR = 0.1041 for 2093 observed reflections (I > 2σ(I)); Compound 2 crystallizes in monoclinic, space group P21/c with a = 11.4042(12), b = 10.9481(11), c = 11.6722(12) ?, β = 99.948(2)o, V = 1435.4(3) ?3, Z = 2, Dc = 2.794 g/cm3, Mr = 1207.80, μ(MoKα) = 3.223 mm-1, F(000) = 1160, the final R = 0.0544 and wR = 0.1066 for 1906 observed reflections (I > 2σ(I)). Both compounds 1 and 2 adopt the Anderson structure, in which the anion is of centrosymmetry and formed by six octahedral edge-sharing MoO6units surrounding the central MO6 (M = Mn or Co) octahedron.
基金The project was supported by the 973 program of the MOST (001CB108906) the NNSFC (90206040+4 种基金 20073048) the NSF ofFujian Province 2002F015 2002J006) the State Key Lab of Structural Chemistry (030065) and the Chinese Academy of Sciences
文摘The title compound, {Mn(H2O)4(VO)2(PO4)2}n 1, was synthesized by the hydro- thermal reaction of Mn(OAc)2, Na2VO3 and H3PO4 in aqueous solution and its crystal structure was determined by X-ray single-crystal analysis. Crystallographic data for 1: H4MnO14P2V2, tetragonal system, space group I4/mmm, a = 6.251(3), c = 13.410(9) ?, Mr = 446.79, V = 524.0(5) ?3, Z = 2, F(000) = 434, μ = 3.320 mm-1, Dc = 2.832 g/cm3, the final R = 0.0577 for 163 observed reflections (I > 2σ(I)). X-ray crystal structure analysis shows that the vanadium phosphorous oxide layers are further connected by MnII(H2O)4 cations to form a three-dimensional network.