Co(en) 3V 3O 6·H 2O has been synthesized by using hydrothermal method and characterized by IR, ICP, XPS and X ray diffraction analysis. The results of the X ray diffraction analysis show that structure of Co(en) ...Co(en) 3V 3O 6·H 2O has been synthesized by using hydrothermal method and characterized by IR, ICP, XPS and X ray diffraction analysis. The results of the X ray diffraction analysis show that structure of Co(en) 3(VO 3) 3·H 2O is orthorhombic with P2(1)2(1)2(1) , and the crystal data are a =0 819 2(7) nm, b =1.263 9(1) nm, c =1.804 8(2) nm, V =1.868 8(3) nm 3, Z=4, D c=1.973 g/cm 3, F (000)=1 124, R 1=0.040 7, wR 2=0.094 9, ( Δ/ρ ) max =706 e/nm 3 and ( Δ/ρ ) min =-452 e/nm 3. The results of XPS show that the Co 2+ was oxidized to Co 3+ (en) 3 at about pH=7.0 in the aqueous solution.展开更多
The new oxovanadium(V)complex,[PyH][VO2(L)]1(salicyladehyde 5-bromo salicyloylhydrazone is abbreviated as H2L;Hpy is protonated pyridine)was obtained from a refluxed solution of VOSO4 and H2L in acetonitrile-methanol-...The new oxovanadium(V)complex,[PyH][VO2(L)]1(salicyladehyde 5-bromo salicyloylhydrazone is abbreviated as H2L;Hpy is protonated pyridine)was obtained from a refluxed solution of VOSO4 and H2L in acetonitrile-methanol-pyridine.Similarly,another new complex,[VO(L)(OCH3)]2 was synthesized by refluxing VOSO4 and H2L in methanol-pyridine.Crystal data for 1:C19H15N3O5BrV,Mr=496.2,monoclinic,P21/n,a=7.1885(3),b=9.2718(3),c=28.803(1)A,β=96.185(1)°,Z=4and V=1908.6(1)A^3;for 2:C15H12N2O5BrV,Mr=431.1,monoclinic ,P21/n,a=12.202(2),b=8.045(2),c=16.604(3)A,β=101.29(3)°,Z=4 and V=1598.4(2)A^3.The structures of 1 and 2 have been determined by X-ray analyses and reveal that the coordination environments of V atoms in both complexes are of square-based pyramid.Three of the four based donor atoms are from the tridentate“ONO”donor ligand while the fourth is one terminal oxygen atom with the V(1)-O(3)distance 1.646(4)Afor 1 and one-OCH3 group with the V(1)-O(3) distance 1.753(3)Afor 2.The V(1)-O(4) terminals occupy the axial sites in both cases.The complexes are also characterized by IR and ^1HNMR spectroscopies.展开更多
文摘Co(en) 3V 3O 6·H 2O has been synthesized by using hydrothermal method and characterized by IR, ICP, XPS and X ray diffraction analysis. The results of the X ray diffraction analysis show that structure of Co(en) 3(VO 3) 3·H 2O is orthorhombic with P2(1)2(1)2(1) , and the crystal data are a =0 819 2(7) nm, b =1.263 9(1) nm, c =1.804 8(2) nm, V =1.868 8(3) nm 3, Z=4, D c=1.973 g/cm 3, F (000)=1 124, R 1=0.040 7, wR 2=0.094 9, ( Δ/ρ ) max =706 e/nm 3 and ( Δ/ρ ) min =-452 e/nm 3. The results of XPS show that the Co 2+ was oxidized to Co 3+ (en) 3 at about pH=7.0 in the aqueous solution.
基金supported by the National Natural Science Foundation of China(21876168,21507130)the Key Projects for Common Key Technology Innovation in Key Industries in Chongqing(cstc2016zdcy-ztzx0020-01)+2 种基金the Chongqing Science&Technology Commission(cstc2016jcyjA0070,cstckjcxljrc13)the Open Project Program of Chongqing Key Laboratory of Catalysis and Functional Organic Molecules from Chongqing Technology and Business University(1456029)the Graduate Innovation Project of Chongqing Technology and Business University(yjscxx201803-028-22)~~
基金The work was supported by the Chinese Academy of Sciences, the National Natural Science Foundation of China(20073048)the NSF of Fujian province for financial support
文摘The new oxovanadium(V)complex,[PyH][VO2(L)]1(salicyladehyde 5-bromo salicyloylhydrazone is abbreviated as H2L;Hpy is protonated pyridine)was obtained from a refluxed solution of VOSO4 and H2L in acetonitrile-methanol-pyridine.Similarly,another new complex,[VO(L)(OCH3)]2 was synthesized by refluxing VOSO4 and H2L in methanol-pyridine.Crystal data for 1:C19H15N3O5BrV,Mr=496.2,monoclinic,P21/n,a=7.1885(3),b=9.2718(3),c=28.803(1)A,β=96.185(1)°,Z=4and V=1908.6(1)A^3;for 2:C15H12N2O5BrV,Mr=431.1,monoclinic ,P21/n,a=12.202(2),b=8.045(2),c=16.604(3)A,β=101.29(3)°,Z=4 and V=1598.4(2)A^3.The structures of 1 and 2 have been determined by X-ray analyses and reveal that the coordination environments of V atoms in both complexes are of square-based pyramid.Three of the four based donor atoms are from the tridentate“ONO”donor ligand while the fourth is one terminal oxygen atom with the V(1)-O(3)distance 1.646(4)Afor 1 and one-OCH3 group with the V(1)-O(3) distance 1.753(3)Afor 2.The V(1)-O(4) terminals occupy the axial sites in both cases.The complexes are also characterized by IR and ^1HNMR spectroscopies.
