A novel inorganic-organic hybrid based on isopolyanion,{[Cu2(phen)2(μ-ox)][H2Mo8O26]}·4EtOH·Et2O(1) (phen=phenanthroline,ox=oxalate),was synthesized under open-air mild reaction conditions,and chara...A novel inorganic-organic hybrid based on isopolyanion,{[Cu2(phen)2(μ-ox)][H2Mo8O26]}·4EtOH·Et2O(1) (phen=phenanthroline,ox=oxalate),was synthesized under open-air mild reaction conditions,and characterized by elemental analysis,IR,ICP,TG and single crystal X-ray diffraction analysis.The crystal structure belongs to triclinic system with space group Pī and cell parameters:a=1.1075(5) nm,b=1.1608(5) nm,c=1.3333(5) nm,α=91.683(5)o,β=113.996(5)o,γ=112.170(5)o,V=1.4159(10) nm3,Mr=2017.44,Z=1,Dc=2.366 g/cm3 and F(000)=980.0.The structure of hybrid 1 is a 1D chain constructed of alternating octamolybdate isopolyanions [β-(Mo8O26)4-] and oxalato-bridged dinuclear copper complex cations [Cu2(phen)2(μ-ox)]2+.Ultimately,a 3D supramolecular network was formed by hydrogen bond interactions among the adjacent chains.The result shows that hybrid 1 is the first example of inorganic-organic hybrid constructed from isopolyanion and oxalato-bridged dinuclear copper complex fragment (CCDC No.665101).展开更多
A new Zn(II) phosphonate complex, [Zn3(PhPO3)2(PhPO3H)2(Phen)2]n (Phen = 1,10-phenanthroline), has been synthesized and structurally determined by X-ray single-crystal diffraction. The complex crystallizes i...A new Zn(II) phosphonate complex, [Zn3(PhPO3)2(PhPO3H)2(Phen)2]n (Phen = 1,10-phenanthroline), has been synthesized and structurally determined by X-ray single-crystal diffraction. The complex crystallizes in the monoclinic system, space group C2/c with a = 14.997(3), b = 18.108(4), c = 17.237(3) A, β = 96.61(3)°, V = 4649.9(16) A3, Z = 4, C48H38N4O12P4Zn3, Mr = 1182.87, Dc = 1.690 g/cm3^,μ = 1.743 mm^-1, F(000) = 2400, the final R = 0.0363 and wR = 0.0963. In the structure, the connectivity between two 5-coordinated Zn(II) atoms and four phosphonates as well as two Phen ligands form a Zn2(PhPO3H)2(PhPO3)2(Phen)2 unit, and such a neighboring unit is bridged by 4-coordinated Zn(II) to give rise to a 1D chain along the c axis. The π-π stacking interactions between Phen rings assemble adjacent chains packed together to form a 3D supermolecular architecture.展开更多
Three novel vanadium selenites with the formulae [(VO2)(1,10-phenanthtoline)(SeO3H)]2 1, [(VO2)(2,2′-bipyridine)]2(SeO3) 2 and [(VO)(H2O)(SeO3)2]2(HaEDD) 3 (EDD = N1,N1′-(ethane-1,2-diyl)dieth...Three novel vanadium selenites with the formulae [(VO2)(1,10-phenanthtoline)(SeO3H)]2 1, [(VO2)(2,2′-bipyridine)]2(SeO3) 2 and [(VO)(H2O)(SeO3)2]2(HaEDD) 3 (EDD = N1,N1′-(ethane-1,2-diyl)diethane-1,2-diamine) were hydrothermally synthesized, and characterized with elemental analysis, FT-IR spectrum, Raman spectrum, TG-DTA analysis, EPR spectra, and single-crystal X-ray diffraction analysis. Compound I belongs to the triclinic system, space group P1^- with a = 7.7527(5), b = 9.5345(10), c = 9.8192(8) A^°, α = 92.712(3), β = 105.540(3), γ = 108.154(4)°, V = 657.66(1) A^°^3, Mr = 782.22, Z = 1, F(000) = 384,μ(MoKa) = 3.544 mm^-1, R = 0.0432 and wR = 0.1142; Compound 2 is of orthorhombic system, space group F212121 with a = 7.6574(15), b = 14.916(3), c = 19.085(4) A, V = 2179.8(8) Aa, Mr = 605.21, Z = 4, F(000) = 1200, μ(MoKa) = 2.579 mm^-1, R = 0.0338 and wR = 0.0658; Compound 3 belongs to the triclinic system, space group P1^- with a = 9.247(2), b = 9.659(2), c = 7.2651(19) A^°, α = 98.171(7), β = 103.709(5), γ = 114.712(13)°, V = 550.9(2) A^°^3, Mr = 828.03, Z = 1, F(000) = 400, μ(MoKa) = 7.537 mm^-1, R = 0.0641 and wR = 0.2118. Compound 1 is constructed from alternating corner-shared [VO4N2] octahedra and SeO3H units, forming a dimeric vanadium unit. These assemblies are further linked into an infinite chain via hydrogen bonds along the a axis. In the structure of 2, two distinct V centers form centrosymmetric [V2O6N4] clusters through edge-sharing, and the SeO3 unit serves as a capping unit to fix the oxovanadate cluster. In the structure of 3, each [VO6] octahedron shares four oxygen atoms with adjacent Se atoms, while every SeO3 unit shares two oxygen atoms with neighboring V atoms. This connectivity of alternating VO6 and SeO3 units results in a joint-like chain. Based on the TGA analysis, these three compounds are thermally stable under 200℃ .展开更多
基金Supported by the National Natural Science Foundation of China(No.20871022)Natural Science Foundation of Liaoning Province,China(No.20061073)
文摘A novel inorganic-organic hybrid based on isopolyanion,{[Cu2(phen)2(μ-ox)][H2Mo8O26]}·4EtOH·Et2O(1) (phen=phenanthroline,ox=oxalate),was synthesized under open-air mild reaction conditions,and characterized by elemental analysis,IR,ICP,TG and single crystal X-ray diffraction analysis.The crystal structure belongs to triclinic system with space group Pī and cell parameters:a=1.1075(5) nm,b=1.1608(5) nm,c=1.3333(5) nm,α=91.683(5)o,β=113.996(5)o,γ=112.170(5)o,V=1.4159(10) nm3,Mr=2017.44,Z=1,Dc=2.366 g/cm3 and F(000)=980.0.The structure of hybrid 1 is a 1D chain constructed of alternating octamolybdate isopolyanions [β-(Mo8O26)4-] and oxalato-bridged dinuclear copper complex cations [Cu2(phen)2(μ-ox)]2+.Ultimately,a 3D supramolecular network was formed by hydrogen bond interactions among the adjacent chains.The result shows that hybrid 1 is the first example of inorganic-organic hybrid constructed from isopolyanion and oxalato-bridged dinuclear copper complex fragment (CCDC No.665101).
基金supported by the State Key Laboratory of Structural Chemistry,and the Young Talent Programmed of Fujian Province (No 2006F3072)
文摘A new Zn(II) phosphonate complex, [Zn3(PhPO3)2(PhPO3H)2(Phen)2]n (Phen = 1,10-phenanthroline), has been synthesized and structurally determined by X-ray single-crystal diffraction. The complex crystallizes in the monoclinic system, space group C2/c with a = 14.997(3), b = 18.108(4), c = 17.237(3) A, β = 96.61(3)°, V = 4649.9(16) A3, Z = 4, C48H38N4O12P4Zn3, Mr = 1182.87, Dc = 1.690 g/cm3^,μ = 1.743 mm^-1, F(000) = 2400, the final R = 0.0363 and wR = 0.0963. In the structure, the connectivity between two 5-coordinated Zn(II) atoms and four phosphonates as well as two Phen ligands form a Zn2(PhPO3H)2(PhPO3)2(Phen)2 unit, and such a neighboring unit is bridged by 4-coordinated Zn(II) to give rise to a 1D chain along the c axis. The π-π stacking interactions between Phen rings assemble adjacent chains packed together to form a 3D supermolecular architecture.
基金Supported by the Natural Science Foundation of Henan Institute of Science and Technology (No. 06038)
文摘Three novel vanadium selenites with the formulae [(VO2)(1,10-phenanthtoline)(SeO3H)]2 1, [(VO2)(2,2′-bipyridine)]2(SeO3) 2 and [(VO)(H2O)(SeO3)2]2(HaEDD) 3 (EDD = N1,N1′-(ethane-1,2-diyl)diethane-1,2-diamine) were hydrothermally synthesized, and characterized with elemental analysis, FT-IR spectrum, Raman spectrum, TG-DTA analysis, EPR spectra, and single-crystal X-ray diffraction analysis. Compound I belongs to the triclinic system, space group P1^- with a = 7.7527(5), b = 9.5345(10), c = 9.8192(8) A^°, α = 92.712(3), β = 105.540(3), γ = 108.154(4)°, V = 657.66(1) A^°^3, Mr = 782.22, Z = 1, F(000) = 384,μ(MoKa) = 3.544 mm^-1, R = 0.0432 and wR = 0.1142; Compound 2 is of orthorhombic system, space group F212121 with a = 7.6574(15), b = 14.916(3), c = 19.085(4) A, V = 2179.8(8) Aa, Mr = 605.21, Z = 4, F(000) = 1200, μ(MoKa) = 2.579 mm^-1, R = 0.0338 and wR = 0.0658; Compound 3 belongs to the triclinic system, space group P1^- with a = 9.247(2), b = 9.659(2), c = 7.2651(19) A^°, α = 98.171(7), β = 103.709(5), γ = 114.712(13)°, V = 550.9(2) A^°^3, Mr = 828.03, Z = 1, F(000) = 400, μ(MoKa) = 7.537 mm^-1, R = 0.0641 and wR = 0.2118. Compound 1 is constructed from alternating corner-shared [VO4N2] octahedra and SeO3H units, forming a dimeric vanadium unit. These assemblies are further linked into an infinite chain via hydrogen bonds along the a axis. In the structure of 2, two distinct V centers form centrosymmetric [V2O6N4] clusters through edge-sharing, and the SeO3 unit serves as a capping unit to fix the oxovanadate cluster. In the structure of 3, each [VO6] octahedron shares four oxygen atoms with adjacent Se atoms, while every SeO3 unit shares two oxygen atoms with neighboring V atoms. This connectivity of alternating VO6 and SeO3 units results in a joint-like chain. Based on the TGA analysis, these three compounds are thermally stable under 200℃ .